CN108548852A - A kind of graphene-based film-type hydrogen gas sensor and preparation method thereof - Google Patents
A kind of graphene-based film-type hydrogen gas sensor and preparation method thereof Download PDFInfo
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- CN108548852A CN108548852A CN201810678756.XA CN201810678756A CN108548852A CN 108548852 A CN108548852 A CN 108548852A CN 201810678756 A CN201810678756 A CN 201810678756A CN 108548852 A CN108548852 A CN 108548852A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—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
Abstract
The present invention provides a kind of preparation method of graphene-based film-type hydrogen gas sensor, including：Contact electrode is prepared in the substrate that surface is equipped with graphene film, then two contact electrodes are removed and surround the graphene film other than region, catalyticing metal particle is loaded on graphene film by photoetching, deposition and stripping technology again, hydrogen sensitive resistance unit is obtained, the catalyticing metal particle is discrete distribution and size is 1~10nm.The present invention obtains graphene-based film-type hydrogen gas sensor by the means of micro-nano technology, the preparation method can prepare multiple hydrogen gas sensors simultaneously, it is simple for process, the period is short, at low cost, the product quality of acquisition is stable, low in energy consumption, have to hydrogen highly selective and highly sensitive, hydrogen volume Concentration Testing ranging from 0.0001%~100%, application range is wide.
Description
Technical field
The present invention relates to hydrogen gas sensor field more particularly to a kind of graphene-based film-type hydrogen gas sensor and its preparations
Method.
Background technology
Hydrogen is the main raw material of industry, is most important special gas, in Ferrous Metallurgy, petrochemical industry, traffic fortune
Very extensive application is suffered from defeated, semiconductor, electric power and Gas Industry, it is considered to be the following most important cleaning energy
One of source.But hydrogen also has danger, its colorless and odorless and with wide explosive range (4-75%) and lower
Fiery energy (0.019mJ), while its flame propagation velocity is quickly.Due to the molecule very little of hydrogen, so in actual production, transport
It is easier to reveal with hydrogen in application process.The leakage of hydrogen is the one of the major reasons of safety accidents such as set off an explosion, therefore
The density of hydrogen in environment is detected in actual production and living and is had great importance to the leakage of monitoring hydrogen.
Hydrogen gas sensor is the important tool for detecting the leakage of density of hydrogen monitoring hydrogen, and traditional hydrogen gas sensor generally wraps
Include metal-oxide hydrogen gas sensor, the hydrogen gas sensor of MOS capacitor structure and metal thin film resistor type hydrogen gas sensor
Deng.But there is also this some drawbacks for these sensors：
1) traditional metal-oxide hydrogen gas sensor needs more harsh application conditions, be at a higher temperature
Operation, energy consumption is higher and selectivity is low；
2) MOS capacitor structure hydrogen gas sensor includes detecting element, testing element, reference elements etc., have than
More complex production technology and higher production cost；
3) hydrogen gas sensor of metal thin film resistor type usually requires higher using a large amount of noble metal cost, due in work
Have inherent instability so as to shorten scalar period at a temperature of work, and very for the sensitivity of the hydrogen of small concentration
Low, signal-to-noise ratio is also relatively low.
In recent years, grapheme material arouses widespread concern.It, which is the one kind being stripped out from graphite, has
The nano material of single layer of carbon atom thickness.Graphene is currently known in the world most thin material, its thickness is only one
The diameter (0.142nm) of carbon atom.Although it is material most thin in the world, the intensity of graphene is unexpectedly than in the world most
Taller 100 times good of steel.Graphene also has many excellent physicochemical properties, such as large specific surface area, good
Electric conductivity, excellent chemical stability and outstanding thermal stability.Based on these above-mentioned characteristics, grapheme material is also applied
In sensor field.
But graphene-based sensor is prepared at present and generally uses chemical etching method or mechanical stripping method, these methods
Obtained sensor selectivity and sensitivity need to be improved, and limits the application and development of graphene-based sensor.
Invention content
In view of the problems of the existing technology, a kind of graphene-based film-type hydrogen gas sensor of present invention offer and its preparation
Method, preparation method of the invention keep product quality controllable, and obtained hydrogen gas sensor has higher selectivity and sensitivity.
A kind of preparation method of graphene-based film-type hydrogen gas sensor provided by the invention, including：It is equipped with stone on surface
Contact electrode is prepared in the substrate of black alkene film, then it is thin to surround the graphene other than region for two contact electrodes of removal
Film, then catalyticing metal particle is loaded on graphene film by photoetching, deposition and stripping technology, obtain hydrogen sensitive resistance
Unit, the catalyticing metal particle is discrete distribution and size is 1~10nm.
In above-mentioned technical proposal, catalyticing metal particle is loaded to by graphene film by photoetching, deposition and stripping technology
On, this method prepares effect and is better than existing chemical etching method and mechanical stripping method, and obtained catalyticing metal particle is nanoscale
And size is controllable, improves the sensitivity of hydrogen gas sensor, and can be mass, at low cost, product quality is stablized.
Preferably, the catalyticing metal particle is the binary or ternary alloy of palladium, nickel, platinum or its composition.
In above-mentioned technical proposal, palladium, nickel, platinum or its binary or ternary alloy formed are stronger to the suction-operated of hydrogen,
Wherein palladium and palladium-nickel alloy is better.In addition, after replacing the type of catalyticing metal particle, can be made for gas with various
Sensor.
Preferably, the length of the contact electrode is 50~100 μm, and two interelectrode distances of contact are 10~20
μm。
In above-mentioned technical proposal, contacts the length of electrode and two contact the distance between electrode and determine as conduction
The size of the graphene film of raceway groove determines the resistance value of hydrogen sensitive resistance unit, when size Control is in above range
It is interior, it can realize the high sensitivity to hydrogen and reduce power consumption.
Preferably, the contact electrode is prepared by photoetching, deposition and stripping technology.It carries out preparing contact electricity in this way
Pole size is controllable.
Preferably, the contact electrode is titanium composite layer, and bottom is titanium, and thickness is 10~20nm, and upper layer is gold, thickness
For 40~60nm.
In above-mentioned technical proposal, contact electrode selects titanium composite layer, bottom titanium that can well stick with graphene film
Together, upper layer Jin Buyi is aoxidized, and the thickness of titanium and gold is controlled within the above range respectively, is integrally imitated as contact electrode
Fruit is best.
Preferably, graphene number of plies is 1~10 layer in the graphene film.Reducing graphene number of plies reduces graphene
Film thickness is conducive to improve sensitivity and the resolution ratio of sensor.
Preferably, the preparation method further includes preparing electric signal transmission unit, institute using photoetching, deposition and stripping technology
Electric signal transmission unit is stated to connect with external circuit for the hydrogen sensitive resistance unit.
Preferably, the preparation method further includes preparing protective layer on the surface of the hydrogen sensitive resistance unit, described
Protective layer uses electric insulating medium.
In above-mentioned technical proposal, protective layer can prevent gas penetrate and the particulate matter of dust class from penetrating, it is miscellaneous to prevent
Matter interference signal, while catalytic metal can be protected again, improve stability.
Preferably, the protective layer uses yttrium oxide and/or silica, the yttrium oxide of more preferably 3~5nm of bottom to add
Upper layer 200~300nm silica.
Preferably, the preparation of the protective layer uses photoetching, deposition, thermal oxide and stripping technology.Using the preparation method
Batch production can be realized by preparing protective layer, and hardly be had an impact to hydrogen sensitive resistance unit property in production process.
A kind of preparation method of graphene-based film-type hydrogen gas sensor as a preferred implementation manner, including it is following
Step：
(1) contact electrode mask pattern is prepared in the substrate equipped with graphene film using photoetching process and electric signal passes
Defeated unit mask pattern deposits titanium complex metal layer by sputtering or electron beam coating process, and then stripping cleaning makes
Contact electrode and electric signal transmission unit；
(2) photoetching process is utilized to make etched portions mask pattern, etched portions are contact electrode and two contact electrodes
Between part other than region, etched using oxygen plasma lithographic technique, extra graphene other than removal contact electrode；
(3) catalyticing metal particle mask pattern is made between contacting electrode using photoetching process, use electron beam plated film
In graphene film area load catalyticing metal particle, then stripping cleaning obtains hydrogen sensitive resistance unit；
(4) it uses photoetching process to make protective layer mask pattern, metallic yttrium, high-temperature oxydation is plated using electron beam film plating process
After reuse plasma reinforced chemical vapour deposition silica, then stripping cleaning prepare protective layer.
The present invention also provides the graphene-based film-type hydrogen gas sensors that above-mentioned preparation method is prepared.
The preparation method of the present invention obtains graphene-based film-type hydrogen gas sensor, the preparation by the means of micro-nano technology
Method can prepare multiple hydrogen gas sensors simultaneously, and preparation process is simple, the period is short, at low cost, the product quality stabilization of acquisition,
It is low in energy consumption.As a result of photoetching, deposition and stripping technology in the present invention, obtained discrete type catalyticing metal particle is nanoscale
And size is controllable, has good adhesion with graphene, catalytic activity is high, can respond, need not heat under room temperature
The i.e. detectable hydrogen of element, has highly selective and highly sensitive, hydrogen volume Concentration Testing ranging from 0.0001% to hydrogen
~100%, application range is wide.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is the present invention
Some embodiments for those of ordinary skill in the art without creative efforts, can also basis
These attached drawings obtain other attached drawings.
Fig. 1 is the structural schematic diagram of graphene-based film-type hydrogen gas sensor obtained in the embodiment of the present invention.
Specific implementation mode
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art
The every other embodiment obtained without creative efforts, shall fall within the protection scope of the present invention.
Embodiment 1
The present embodiment provides a kind of preparations of graphene-based film-type hydrogen gas sensor (its structural schematic diagram is as shown in Figure 1)
Method specifically includes following steps：
(1) graphene film 21 being grown on copper foil is transferred in the silicon chip substrate 1 of single side oxidation, then 150
1-2h is toasted in DEG C baking oven or hot plate, the graphene film 21 is single-layer graphene；
(2) contact 23 mask pattern of electrode and the (packet of electric signal transmission unit 3 are prepared on the base 1 using photoetching process
Include metal connecting line 31 and pad 32) mask pattern, titanium complex metal layer is deposited by sputtering or electron beam coating process, so
Stripping cleaning afterwards makes contact electrode 23 and metal connecting line 31 and pad 32；
Wherein, contact electrode 23 grows 50 μm, and 5 μm wide, the distance between two contact electrodes 23 are 10 μm；Titanium composite layer
Bottom be titanium, thickness be 10~20nm, upper layer be gold, thickness be 40~60nm.
(3) photoetching process is utilized to make etched portions mask pattern, etched portions are contact electrode 23 and two contact electricity
The part other than region between pole 23, is etched using oxygen plasma lithographic technique, extra stone other than removal contact electrode 23
Black alkene；
(4) it uses photoetching process to make the mask pattern of catalyticing metal particle 22 between contacting electrode 23, uses electronics
Beam plated film is in 21 area load catalyticing metal particle 22 of graphene film, and catalyticing metal particle 22 is palladium, grain size 1nm, in from
Type distribution is dissipated, then stripping cleaning obtains hydrogen sensitive resistance unit 2；
(5) photoetching process is used to make 4 mask pattern of protective layer, electron beam film plating process plates metallic yttrium, thickness 3-
5nm, then 200 DEG C of oxidation 30min, reuse plasma reinforced chemical vapour deposition silica, thickness 200-300nm,
Then protective layer 4 is prepared in stripping cleaning；
(6) graphene-based film-type hydrogen gas sensor is obtained finally by scribing sliver technique.
Multiple hydrogen gas sensors can be prepared simultaneously by above-mentioned preparation method, and preparation process is simple, and the period is short, can batch
Production, at low cost, the product function stabilization of acquisition, power consumption are relatively low.
The method that density of hydrogen is tested using the graphene-based film-type hydrogen gas sensor in the present embodiment is as follows：
(1) graphene-based film-type hydrogen gas sensor is fixed on test board, test board be comprising pad and with outside
Then the wire PCB plate of connection will be fixed with hydrogen by the pad on hydrogen gas sensor together with the pad solder of test board
The test board of gas sensor is put into the atmosphere containing a certain concentration hydrogen, and environmental condition keeps homogeneous constant；
It is constant that the environment homogeneous constant refers to that the gas in atmosphere is evenly distributed, and the temperature humidity of environment is equal
It is even constant, avoid environmental fluctuating from having an impact device.
(2) resistance variations of hydrogen gas sensor are tested by the conducting wire on test board to detect density of hydrogen, the electricity
Hinder variable quantity and the proportional relationship of environment density of hydrogen.
Hydrogen high sensitivity is detected with the hydrogen gas sensor in the present embodiment, detection limit is low, when hydrogen volume concentration only has
When 0.0001%, can also it be detected.
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, it will be understood by those of ordinary skill in the art that：It still may be used
With technical scheme described in the above embodiments is modified or equivalent replacement of some of the technical features；
And these modifications or replacements, various embodiments of the present invention technical solution that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (10)
1. a kind of preparation method of graphene-based film-type hydrogen gas sensor, which is characterized in that including：It is equipped with graphene on surface
Contact electrode is prepared in the substrate of film, is then removed two contact electrodes and is surrounded the graphene film other than region, then
Catalyticing metal particle is loaded on graphene film by photoetching, deposition and stripping technology, obtains hydrogen sensitive resistance unit,
The catalyticing metal particle is discrete distribution and size is 1~10nm.
2. preparation method according to claim 1, which is characterized in that the catalyticing metal particle is palladium, nickel, platinum or its group
At binary or ternary alloy.
3. preparation method according to claim 1 or 2, which is characterized in that the length of the contact electrode is 50~100 μ
M, two interelectrode distances of contact are 10~20 μm.
4. preparation method according to claim 1, which is characterized in that described in the preparation of photoetching, deposition and stripping technology
Contact electrode；The contact electrode is titanium composite layer, and bottom is titanium, and thickness is 10~20nm, and upper layer is gold, thickness is 40~
60nm。
5. preparation method according to claim 1, which is characterized in that in the graphene film graphene number of plies be 1~
10 layers.
6. preparation method according to claim 1, which is characterized in that further include using photoetching, deposition and stripping technology system
Standby electric signal transmission unit, the electric signal transmission unit are connect for the hydrogen sensitive resistance unit with external circuit.
7. preparation method according to claim 1 or 6, which is characterized in that further include in the hydrogen sensitive resistance unit
Surface prepare protective layer, the protective layer uses electric insulating medium.
8. preparation method according to claim 7, which is characterized in that the protective layer uses yttrium oxide and/or titanium dioxide
Silicon, the preferably yttrium oxide of 3~5nm of bottom add layer 200~300nm silica.
9. preparation method according to claim 7, which is characterized in that the preparation of the protective layer is using photoetching, deposition, heat
Oxidation and stripping technology.
10. the graphene-based film-type hydrogen gas sensor that claim 1~9 any one of them preparation method is prepared.
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| CN109896499A (en) * | 2019-03-04 | 2019-06-18 | 中国电子科技集团公司第四十九研究所 | A kind of ceramic microstructures graphene gas sensor and its manufacturing method |
| CN110398522A (en) * | 2019-08-28 | 2019-11-01 | 北京智芯微电子科技有限公司 | Integrated gas sensing unit based on graphene and preparation method thereof |
| CN111413373A (en) * | 2020-04-01 | 2020-07-14 | 西安石油大学 | Optical fiber sensor based on graphene-based composite structure and preparation method thereof |
| CN116908248A (en) * | 2023-06-26 | 2023-10-20 | 天津大学 | Hydrogen sensor based on graphene and preparation method thereof |
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| CN109490367A (en) * | 2018-09-30 | 2019-03-19 | 兰州空间技术物理研究所 | A kind of mon-H sensor and preparation method thereof |
| CN109557138A (en) * | 2018-10-25 | 2019-04-02 | 北京镭硼科技有限责任公司 | A kind of graphene-based gas sensing materials of Metal Palladium load and preparation and application |
| CN109896499A (en) * | 2019-03-04 | 2019-06-18 | 中国电子科技集团公司第四十九研究所 | A kind of ceramic microstructures graphene gas sensor and its manufacturing method |
| CN109896499B (en) * | 2019-03-04 | 2021-02-09 | 中国电子科技集团公司第四十九研究所 | Ceramic microstructure graphene gas sensor and manufacturing method thereof |
| CN110398522A (en) * | 2019-08-28 | 2019-11-01 | 北京智芯微电子科技有限公司 | Integrated gas sensing unit based on graphene and preparation method thereof |
| CN111413373A (en) * | 2020-04-01 | 2020-07-14 | 西安石油大学 | Optical fiber sensor based on graphene-based composite structure and preparation method thereof |
| CN111413373B (en) * | 2020-04-01 | 2023-03-31 | 西安石油大学 | Optical fiber sensor based on graphene-based composite structure and preparation method thereof |
| CN116908248A (en) * | 2023-06-26 | 2023-10-20 | 天津大学 | Hydrogen sensor based on graphene and preparation method thereof |
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Application publication date: 20180918 |