CN108303122A - The bionical optical detector of graphene and preparation method thereof based on thermoregulation energy - Google Patents
The bionical optical detector of graphene and preparation method thereof based on thermoregulation energy Download PDFInfo
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- CN108303122A CN108303122A CN201710024581.6A CN201710024581A CN108303122A CN 108303122 A CN108303122 A CN 108303122A CN 201710024581 A CN201710024581 A CN 201710024581A CN 108303122 A CN108303122 A CN 108303122A
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 117
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 116
- 230000003287 optical effect Effects 0.000 title claims abstract description 41
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- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 45
- 239000012528 membrane Substances 0.000 claims abstract description 38
- 239000000758 substrate Substances 0.000 claims abstract description 36
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 10
- 238000000137 annealing Methods 0.000 claims abstract description 7
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 7
- 238000012360 testing method Methods 0.000 claims description 39
- 239000002131 composite material Substances 0.000 claims description 29
- 239000011261 inert gas Substances 0.000 claims description 29
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- 229910052739 hydrogen Inorganic materials 0.000 claims description 22
- 229910052751 metal Inorganic materials 0.000 claims description 19
- 239000002184 metal Substances 0.000 claims description 19
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 14
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 14
- 238000009413 insulation Methods 0.000 claims description 12
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- 230000008569 process Effects 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 4
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 4
- 238000012546 transfer Methods 0.000 claims description 4
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 3
- NQTADLQHYWFPDB-UHFFFAOYSA-N N-Hydroxysuccinimide Chemical compound ON1C(=O)CCC1=O NQTADLQHYWFPDB-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 3
- KQSABULTKYLFEV-UHFFFAOYSA-N naphthalene-1,5-diamine Chemical compound C1=CC=C2C(N)=CC=CC2=C1N KQSABULTKYLFEV-UHFFFAOYSA-N 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- KCYOZNARADAZIZ-CWBQGUJCSA-N 2-[(2e,4e,6e,8e,10e,12e,14e)-15-(4,4,7a-trimethyl-2,5,6,7-tetrahydro-1-benzofuran-2-yl)-6,11-dimethylhexadeca-2,4,6,8,10,12,14-heptaen-2-yl]-4,4,7a-trimethyl-2,5,6,7-tetrahydro-1-benzofuran-6-ol Chemical class O1C2(C)CC(O)CC(C)(C)C2=CC1C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)C1C=C2C(C)(C)CCCC2(C)O1 KCYOZNARADAZIZ-CWBQGUJCSA-N 0.000 claims description 2
- 229910052738 indium Inorganic materials 0.000 claims 1
- BXGTVNLGPMZLAZ-UHFFFAOYSA-N n'-ethylmethanediimine;hydrochloride Chemical class Cl.CCN=C=N BXGTVNLGPMZLAZ-UHFFFAOYSA-N 0.000 claims 1
- 239000010410 layer Substances 0.000 description 54
- 102000005962 receptors Human genes 0.000 description 43
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- 230000000694 effects Effects 0.000 description 9
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- 239000000463 material Substances 0.000 description 7
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 7
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 230000004044 response Effects 0.000 description 5
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- 239000000377 silicon dioxide Substances 0.000 description 5
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- 238000012986 modification Methods 0.000 description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 4
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- 238000000151 deposition Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- -1 for example Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
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- 206010043458 Thirst Diseases 0.000 description 1
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- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
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- 125000000524 functional group Chemical group 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
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- 102000004169 proteins and genes Human genes 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
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- 238000001228 spectrum Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
- 238000001931 thermography Methods 0.000 description 1
- 230000035922 thirst Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
- G01D5/00—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable
- G01D5/26—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable characterised by optical transfer means, i.e. using infrared, visible, or ultraviolet light
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
Abstract
The present invention provides a kind of bionical optical detector of graphene and preparation method thereof based on thermoregulation energy, and the preparation method includes:1) graphene and micro-heater platform are provided, and the graphene is transferred on the micro-heater platform;2) the obtained structure of step 1) is placed in chemical vapour deposition reactor furnace and is annealed;3) graphene surface after annealing is modified by reagent, forms the active film of active group;4) light receptor albumen is formed in the active film surface.The present invention connects graphene by using the heating structure of outstanding membrane type, and modifies light receptor albumen on the surface of graphene, on the one hand light receptor albumen is used to realize wavelength selectivity, improves absorptivity;On the other hand using membrane type heating structure is hanged, influence of the substrate to graphene performance is reduced, more operating temperature can be adjusted by heating voltage, to adjust photo-generated carrier mobility and concentration, to improve the performance of light-detecting device.
Description
Technical field
The invention belongs to technical field of photoelectric detection more particularly to a kind of bionical light of graphene based on thermoregulation energy
Detector and preparation method thereof.
Background technology
Photodetector has a wide range of applications in daily life and military field, and the photodetection of different-waveband
Device has different applications.Ultraviolet band is for observing ground lower atmosphere layer uitraviolet intensity variation and Solar Physics, imminent earthquake
Prediction research etc.;Visible light or near infrared band are used for radionetric survey and detection, industry automatic control, Photometric Measurement etc.;It is infrared
Wave band is for missile guidance, infrared thermal imaging, infrared remote sensing etc..The photodetector of different-waveband, for different field
Important in inhibiting.
A kind of photosensitive biomolecule of light receptor albumen, the wavelength of covering can be had by infrared region to ultraviolet region
Wavelength selectivity is good, the feature high to the fast response time of light, absorptivity.The optical sensor prepared using light receptor albumen will
Has the structure more simpler than conventional photodetectors, less expensive manufacturing cost and higher sensitivity.
The optical detector of traditional semi-conducting material, although haveing excellent performance, material preparation is difficult, and is wanted to working environment
Ask high, detector is of high cost.Graphene as a kind of unique two-dimensional material, at room temperature with superelevation carrier mobility,
The optical absorption spectra of ultra-wide (from ultraviolet to far infrared) so that it is great in terms of the low cost optical detection for realizing high speed, wide spectrum
Potentiality.In addition, the specific surface area of graphene superelevation and excellent electric conductivity become in the redox of enzyme or protein
Good electron propagation ducts between the heart and electrode surface.By to graphene modified target molecule, can quickly transmit electronics,
The selective enumeration method of biomolecule can be realized again, therefore graphene is also the ideal material for preparing biosensor.
But there is also apparent disadvantages for optical detection for graphene:Intrinsic graphene is low to the absorptivity of light, lacks light
Gain mechanism causes the photoresponse rate of device relatively low;The photo-generated carrier short life of graphene itself, only picoseconds, cause
Photo-generated carrier is difficult to effectively collect, and also seriously affects the photoresponse rate of detector, the low-response rate of graphene detector can not
Meet the needs of practical application.In addition, substrate material can significantly affect the property of graphene, for example, SiO2Substrate it is not pure and mild
Phonon vibration can lead to carrier scattering in graphene, the serious mobility for reducing graphene carrier;Graphene phonon and lining
The interaction of bottom phonon makes its thermoelectricity conductance reduce 1/5th of intrinsic graphene.Therefore, the mobility of carrier is improved
It is significant to graphene optical detection.
Therefore, concentration, the mobility of photo-generated carrier how are simply and efficiently improved, the sensitivity for improving device is this
The technical staff in field thirsts for the technical barrier solved.
Invention content
In view of prior art described above disadvantage, it is imitative using temperature adjusting graphene that the purpose of the present invention is to provide a kind of
The method of third contact of a total solar or lunar eclipse detector performance, to solve at this stage, graphene optical detector is low to the absorptivity of light, sensitivity is low asks
Topic.
In order to achieve the above objects and other related objects, it is imitative to provide a kind of graphene based on thermoregulation energy by the present invention
The preparation method of third contact of a total solar or lunar eclipse detector, which is characterized in that include the following steps:
1) graphene and micro-heater platform are provided, and the graphene is transferred on the micro-heater platform;
2) structure that step 1) obtains is placed in chemical vapour deposition reactor furnace and is annealed;
3) graphene surface after annealing is modified using reagent, to have in graphene surface formation
The active film of active group;
4) light receptor albumen, the activity of the light receptor albumen and the active film are formed in the active film surface
Group combines and forms covalent bond, to connect the light receptor albumen and the active film.
As a preferred embodiment of the present invention, in step 1), the micro-heater platform is made of following steps:
A substrate 1-1) is provided, and in forming composite membrane on the substrate, the composite membrane is for defining heating film region
With supporting beam area;
1-2) in formation heating metal layer on the composite membrane, and by the heating metallic layer graphic to obtain resistor
Part, the resistance device include resistive heater, first for electrical lead, the first current electrode, at least described resistive heater position
In the heating film region;
1-3) in forming insulating layer on the heating metal layer;
1-4) in formation test metal layer on the insulating layer, and by the test metallic layer graphic to obtain electrode device
Part, the electrode device include test electrode, second for electrical lead, the second current electrode, at least described test electrode with it is described
Resistive heater is correspondingly arranged up and down, in addition, the graphene at least covers the test electrode;
1-5) in step 1-4) film release window is formed in the structure that is formed, and expose the substrate;
Heat-insulation chamber 1-6) is formed by substrate described in the film release window erodable section, to release the heating film
Area and supporting beam area.
As a preferred embodiment of the present invention, step 1-1) in, the substrate is the silicon substrate in (100) face, described multiple
It is the composite membrane that at least one layer of silicon oxide film and at least one layer of silicon nitride film are formed to close film.
As a preferred embodiment of the present invention, step 1-4) in, the test electrode is interdigital electrode.
As a preferred embodiment of the present invention, step 1-6) in, the shape in the supporting beam area is linear or snakelike.
As a preferred embodiment of the present invention, in step 1), using direct transfer process or PMMA methods by the graphene
It is transferred on the micro-heater platform.
As a preferred embodiment of the present invention, step 2) specifically includes:
2-1) inert gas is used to carry out ventilation and gas exhaust treatment to the reacting furnace;
2-2) inert gas is passed through into the reacting furnace at a temperature of first;
2-3) inert gas and hydrogen are passed through into the reacting furnace simultaneously under second temperature;
The flow of the inert gas and the hydrogen 2-4) is reduced, and is cooled down to the reacting furnace.
As a preferred embodiment of the present invention, step 2-1) in, the flow of the inert gas be 500sccm~
2000sccm, the ventilation and gas exhaust treatment time are 2min~3min;
As a preferred embodiment of the present invention, step 2-2) in, first temperature is 200 DEG C~300 DEG C, described lazy
Property gas flow be 500sccm~2000sccm.
As a preferred embodiment of the present invention, step 2-3) in, the second temperature is 300 DEG C~400 DEG C, and in institute
It is total with the mixed gas of the inert gas to state holding 5min~10min, the hydrogen being passed through after heat preservation under second temperature
Flow 500sccm~2000sccm, the volume fraction of hydrogen described in the mixed gas are 30%~50%, are passed through described lazy
Property gas and the hydrogen time be 40min~120min.
As a preferred embodiment of the present invention, step 2-4) in, the flow 50sccm of the inert gas~
The mode of 200sccm, flow 10sccm~40sccm of the hydrogen, the cooling are reacting furnace Temperature fall.
As a preferred embodiment of the present invention, in step 3), the reagent include 1,5-diaminonaphthalene, 1- pyrenes butyric acid,
Glutaraldehyde, 1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides and one kind in n-hydroxysuccinimide or two
Kind or more combination;The active group is amino active group, carboxyl-reactive group, one kind in aldehyde radical active group or two
Kind or more combination.
As a preferred embodiment of the present invention, in step 4), the light receptor albumen includes opsin class, phytochrome
Class, cryptochrome class, the combination to one or more of photopigment class, BLUF structural domains class, ultraviolet light receptor class.
As a preferred embodiment of the present invention, including:Micro-heater platform;It is flat to be located at the micro-heater for graphene
On platform;Active film is formed in the surface of the graphene;Light receptor albumen is formed on the active film.
As a preferred embodiment of the present invention, the micro-heater platform includes successively from bottom to top:
Substrate, including a heat-insulation chamber;
Composite membrane is located above the heat-insulation chamber, including heating film region and supporting beam area, and the supporting beam area connects institute
State heating film region and the substrate;
Resistance device, including resistive heater, first are for electrical lead, the first current electrode, wherein at least described heating electricity
Resistance silk is formed on the heating film region;
Insulating layer, is formed on the resistance device, at least covers the resistive heater;
Electrode device is formed on the insulating layer, and includes testing electrode, second for electrical lead, the second power supply electricity
Pole, wherein at least described test electrode is correspondingly arranged up and down with the resistive heater, and the graphene at least covers the survey
Try electrode.
As a preferred embodiment of the present invention, the test electrode is interdigital electrode.
As a preferred embodiment of the present invention, the active film is the active film of active group, the light
Receptor protein is combined to form covalent bond with the active group of the active film, to connect the light receptor albumen and the activity
Film.
As described above, the bionical optical detector of graphene and preparation method thereof based on thermoregulation energy of the present invention, tool
It has the advantages that:
1) test electrode of the invention is located at heating film region corresponding section, for connecting graphene, builds built in field, drives
Dynamic photo-generated carrier flowing, so that response signal enhances;
2) it is the temperature needed for sensor provides work to use the heating structure of outstanding membrane type, and reduction substrate is to graphene performance
Influence, and by suspension structures be enriched with heat, be conducive to improve temperature uniformity, be easy to by adjusting and controlling operating temperature
To improve the performance of sensor;
3) it uses light receptor albumen to realize wavelength selectivity, improves absorptivity, solve intrinsic graphene optical detector
The problem of wave band is difficult to differentiate between, and prepare simply, it is of low cost, it is suitable for batch production;
Description of the drawings
Fig. 1 is shown as the system of the bionical optical detector of graphene based on thermoregulation energy of the offer of the embodiment of the present invention one
Preparation Method flow chart.
Fig. 2 a-2l are shown as the bionical optical detection of graphene based on thermoregulation energy provided in the embodiment of the present invention one
Structural schematic diagram in each step of preparation method of device, wherein Fig. 2 h are the sectional view of Fig. 2 i, and Fig. 2 j are the explosion of Fig. 2 i structures
Figure.
Component label instructions
1 micro-heater platform
11 substrates
12 composite membranes
13 heating metal layers
130 resistance devices
131 resistive heaters
132 first for electrical lead
133 first current electrodes
14 insulating layers
15 test metal layers
150 electrode devices
151 test electrodes
152 second for electrical lead
153 second current electrodes
16 film release windows
17 heat-insulation chambers
2 graphenes
3 active groups
4 light receptor albumen
S11~S14 steps
Specific implementation mode
Illustrate that embodiments of the present invention, those skilled in the art can be by this specification below by way of specific specific example
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also be based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under the spirit of the present invention.
It please refers to Fig.1 to Fig. 2 l.It should be noted that the diagram provided in the present embodiment only illustrates this in a schematic way
The basic conception of invention, though package count when only display is with related component in the present invention rather than according to actual implementation in diagram
Mesh, shape and size are drawn, when actual implementation kenel, quantity and the ratio of each component can be a kind of random change, and its
Assembly layout form may also be increasingly complex.
Embodiment one
Referring to Fig. 1, the present invention provides a kind of preparation side of the bionical optical detector of graphene based on thermoregulation energy
Method, which is characterized in that include the following steps:
1) graphene and micro-heater platform are provided, and the graphene is transferred on the micro-heater platform;
2) structure that step 1) obtains is placed in chemical vapour deposition reactor furnace and is annealed;
3) graphene surface after annealing is modified using reagent, to have in graphene surface formation
The active film of active group;
4) light receptor albumen, the activity of the light receptor albumen and the active film are formed in the active film surface
Group combines and forms covalent bond, to connect the light receptor albumen and the active film.
In step 1), the S1 steps in please referring to Fig.1 and Fig. 2 a provide graphene 2 and micro-heater platform 1, and will
The graphene 2 is transferred on the micro-heater platform 1;
Specifically, in the present embodiment, the graphene 2 is single-layer graphene, in other embodiments, or double
Layer or multi-layer graphene.Furthermore it is preferred that the graphene 2 can be but be not limited to the graphene grown on copper-based bottom.Into one
It walks, graphene 2 described in the present embodiment is intrinsic graphene, but is not limited thereto.
As an example, the graphene is transferred to institute using direct transfer process or PMMA (polymethyl methacrylate) methods
It states on electrode device.
Specifically, by taking direct transfer process as an example, the graphene is transferred on the electrode device and is included the following steps:
First, there is the copper-based bottom of the graphene 2 to be placed in etchant solution surface growth and corrode 2h, the etchant solution is one
Determine the Fe (NO of concentration (for example a concentration of 0.1g/ml)3)3Solution or FeCl3Solution makes the graphene 2 and the copper-based bottom point
From;Secondly, the graphene 2 is picked up using micro-heater platform.
Specifically, using Fe (NO3)3Solution or FeCl3After solution makes the graphene 2 be detached with the copper-based bottom, profit
Can also include that the graphene 2 is placed in certain molar concentration before being picked up the graphene 2 with micro-heater platform
Corrode 1h in the HCl solution of (for example molar concentration be 10%), the step of copper to remove 2 remained on surface of the graphene.
Meanwhile the preparation method of micro-heater platform described in step 1) is specially:
Fig. 2 b-2c are please referred to, carry out step 1-1 first), a substrate 11 is provided, and compound in being formed on the substrate 11
Film 12, the composite membrane is for defining heating film region (not shown) and supporting beam area (not shown);
As an example, step 1-1) in, the substrate 11 is the silicon substrate in (100) face, or SOI substrate, to carry
The speed of service etc. of high device inside circuit.The composite membrane 12 is at least one layer of silicon oxide film and at least one layer of silicon nitride film shape
At composite membrane.
Specifically, after the composite membrane 12 is graphical in the subsequent process, the heating film region and supporting beam area are defined.
The composite membrane 12 is using oxidation, plasma enhanced chemical vapor deposition (PECVD) or low-pressure chemical vapor deposition
The methods of (LPCVD) it is formed on the substrate 11.In other embodiments, the composite membrane 12 can also be nitrating it is porous,
Silicon carbide etc., these materials have good self-stopping technology effect to the anisotropic wet corrosion of silicon, in addition, its coefficient of heat conduction is very
Small, the supporting beam area heat-insulating property of making is good, and the thermal losses of generation is relatively low.
Preferably, 12 preparation process of the composite membrane is:First, it is sunk successively using low-pressure chemical vapor deposition (LPCVD)
Product a layer thickness is the silica of 0.1 μm~0.5 μm (the present embodiment is 0.2 μm) and a layer thickness is 0.1 μm~0.5 μm (this
Embodiment be 0.2 μm) silicon nitride;Secondly, plasma enhanced chemical vapor deposition (PECVD) is recycled to be sequentially depositing one layer
Thickness is the silica of 0.1 μm~0.5 μm (the present embodiment is 0.2 μm) and a layer thickness is 0.1 μm~0.5 μm (the present embodiment
Be 0.2 μm) silicon nitride.Further, if the composite membrane is formed by two layers or more silicon oxide film and two layers or more silicon nitride film,
It is preferably then that the silicon oxide film is alternately superimposed on the silicon nitride film.
As an example, the shape in the supporting beam area is linear or snakelike.
Specifically, the length in the supporting beam area can be increased by warp architecture, serpentine design is such as used, is contributed to
Reduce the thermal conductivity in supporting beam area.
Fig. 2 d are please referred to, step 1-2 is carried out), metal layer 13 is heated in being made on the composite membrane 12, and in the heating
Figure dissolves resistance device 130 on metal layer 13, the resistance device include resistive heater 131, first for electrical lead 132,
First current electrode 133;
Specifically, the material of the heating metal layer 13 is Ti/Au or Ti/Pt, the thickness of the heating metal layer 13
For 30nm~300nm, in the present embodiment, the thickness of the heating metal layer 13 is 100nm, in addition, the graphic method
To use lift-off or wet corrosion technique, wherein the resistive heater 131 is preferably snakelike resistive heater, this
Sample can be with its size of reasonable arrangement, and increases the uniformity of Temperature Distribution, or other shapes of resistive heater, herein
It is not limited.In addition, the first electrode lead 132 connects the resistive heater 131 and first current electrode
133, also, the described first surface for being preferably placed at the supporting beam area for electrical lead 132.
Fig. 2 e are please referred to, step 1-3 is carried out), in formation insulating layer 14 on the heating metal layer 13;
Enhance chemical vapor deposition (PECVD) in heating gold specifically, the insulating layer 14 is using plasma
Belong to and makes silicon nitride dielectric layer on layer 13.Wherein, the thickness of the silicon nitride dielectric layer is 400nm~600nm, in the present embodiment
In, preferably 500nm.
Fig. 2 f are please referred to, step 1-4 is carried out), metal layer 15 is tested in being formed on the insulating layer 14, and in the test
Figure dissolves electrode device 150 on metal layer 15, the electrode device 150 include test electrode 151, second for electrical lead 152,
Second current electrode 153, at least described test electrode 151 is correspondingly arranged with about 131 resistive heater, in addition, described
Graphene 2 at least covers the test electrode 151;
As an example, the test electrode 151 is interdigital electrode.
Specifically, the material of the test metal layer 15 is Ti/Au or Ti/Pt, the thickness of the test metal layer 15
For 30nm~300nm, in the present embodiment, the thickness of the test metal layer 15 is 100nm, in addition, the electrode device 150
Forming method be using lift-off or wet corrosion technique.In addition, the second electrode lead 152 connects the test
Electrode 151 and second current electrode 153, also, described second is preferably placed at for electrical lead 152 corresponding to the support
The position of Liang Qu.
Preferably, in the present embodiment, the test electrode 151 is interdigital electrode, wherein the interdigital electrode, which is located at, to be added
Hotting mask area corresponding section builds built in field for connecting graphene, and using interdigital electrode, more effectively photoproduction is driven to carry
It is dynamic to flow subflow, so that response signal enhances, it is of course also possible to for the electrode of other shapes, such as snakelike electrode, herein not
It is restricted.
Please refer to Fig. 2 g, carry out step 1-5), in step 1-4) film release window 16 is formed in the structure that is formed, and reveal
Go out the substrate 11;
Specifically, during forming film release window 16, retain the electrode device (including test electrode
151, second for electrical lead 152, the second current electrode 153) and the resistance device (including resistive heater 131, first supplies
Electrical lead 132, the first current electrode 133), remove the exposed insulating layer 14 and the composite membrane 12.Preferably, in described
Figure dissolves heating film region and supporting beam area in composite membrane 12, the supporting beam area at least support the resistive heater 131 with
And the test electrode 151, and connect the heating film region and the substrate 11;
Fig. 2 h-2j are please referred to, step 1-6 is carried out), pass through 11 shape of substrate described in 16 erodable section of film release window
At heat-insulation chamber 17, to release the heating film region and supporting beam area;
Specifically, step 1-6) in, the substrate 11 is corroded using anisotropic etchant, the anisotropic wet is rotten
Liquid such as tetramethylammonium hydroxide (TMAH) or potassium hydroxide (KOH) etc. are lost, to empty the substrate below the composite membrane 12, release
Go out membrane structure, obtains the device of outstanding membrane type structure.Preferably, the heat-insulation chamber 17 is the heat-insulation chambers such as inverted ladder-shaped body.By upper
State the micro-heater platform with outstanding membrane type heating structure of step formation, it is possible to reduce influence of the substrate to graphene performance,
More operating temperature can be controlled by adjusting heating voltage, to adjust photo-generated carrier mobility and concentration, to improve light
The performance of sensitive detection parts.
It should be noted that using the heating structure (micro-heater platform) of the outstanding membrane type of the offer of the present embodiment two for sensing
Device provides the temperature needed for work, adjusts temperature by changing 131 both end voltage of resistive heater, passes through suspension structures richness
Heat-collecting capacity is conducive to the uniformity for improving temperature, is easy to improve the performance of sensor by adjusting and controlling operating temperature.And
And when light is radiated on the graphene 2 of solidification light receptor albumen 4, the generation of photo-generated carrier is so that the resistance of device becomes
Change, can be achieved with optical detection by measuring the resistance variations between detection electrode.
In step 2), shown in the S12 in please referring to Fig.1, the obtained structure of step 1) is placed in chemical vapor deposition
It anneals in reacting furnace;
As an example, step 2) specifically includes:
2-1) inert gas is used to carry out ventilation and gas exhaust treatment to the reacting furnace;
2-2) inert gas is passed through into the reacting furnace at a temperature of first;
2-3) inert gas and hydrogen are passed through into the reacting furnace simultaneously under second temperature;
The flow of the inert gas and the hydrogen 2-4) is reduced, and is cooled down to the reacting furnace.
Specifically, by above-mentioned annealing process, surface cleaning can be obtained without oxygen-containing functional group in 2 surface of the graphene
The graphene 2.
As an example, step 2-1) in, the flow of the inert gas is 500sccm~2000sccm, the ventilation and
The gas exhaust treatment time is 2min~3min.
Specifically, in the present embodiment, the flow of the inert gas is 1000sccm, when the ventilation and gas exhaust treatment
Between be 2.5min.
As an example, step 2-2) in, first temperature is 200 DEG C~300 DEG C, and the flow of the inert gas is
500sccm~2000sccm.
Specifically, in the present embodiment, first temperature is 250 DEG C, the flow of the inert gas is 1000sccm.
As an example, step 2-3) in, the second temperature is 300 DEG C~400 DEG C, it is preferable that and in second temperature
Degree is lower to keep 5min~10min, the total flow of the hydrogen being passed through after heat preservation and the mixed gas of the inert gas
500sccm~2000sccm, the volume fraction of hydrogen described in the mixed gas are 30%~50%, are passed through the indifferent gas
The time of body and the hydrogen is 40min~120min.
Specifically, in the present embodiment, the second temperature is 350 DEG C, and keeps 8min under the second temperature, is protected
The total flow 1000sccm of the hydrogen being passed through after temperature and the mixed gas of the inert gas, described in the mixed gas
The volume fraction of hydrogen is 40%, and the time for being passed through the inert gas and the hydrogen is 80min.
As an example, step 2-4) in, flow 50sccm~200sccm of the inert gas, the flow of the hydrogen
The mode of 10sccm~40sccm, the cooling are preferably reacting furnace Temperature fall.
Specifically, in the present embodiment, the flow 100sccm of the inert gas, the flow 30sccm of the hydrogen.
In step 3), S13 the and Fig. 2 k in please referring to Fig.1, using reagent to 2 surface of the graphene after annealing into
Row modification, to form the active film (not shown) of active group 3 on 2 surface of the graphene;
As an example, in step 3), the reagent includes 1,5-diaminonaphthalene, 1- pyrenes butyric acid, glutaraldehyde, 1- (3- diformazans
Aminopropyl) one or more of -3- ethyl-carbodiimide hydrochlorides and n-hydroxysuccinimide combination;It is described
Active group is the combination of one or more of amino active group, carboxyl-reactive group, aldehyde radical active group.
Specifically, being handled by mentioned reagent, it is preferred that the available activity with the group ending corresponding to corresponding reagent
Film, in order to connect the light receptor albumen 4.
Specifically, the active group be amino active group, carboxyl-reactive group, one kind in aldehyde radical active group or
Two or more combinations, in other embodiments, or can realize same or analogous with other with this step function
The active film of active group.
In step 4), shown in S14 the and Fig. 2 l in please referring to Fig.1, in active film (not shown) surface
Light receptor albumen 4 is formed, the light receptor albumen 4 is combined to form covalent bond with the active group 3 of the active film, with connection
The light receptor albumen 4 and the active film.
As an example, the light receptor albumen 4 include opsin class light receptor albumen, it is phytochrome class light receptor albumen, hidden
Anthocyan light receptor albumen, to photopigment class light receptor albumen, BLUF structural domain class light receptors albumen, ultraviolet light receptor class light
The combination of one or more of receptor protein.
Specifically, via above-mentioned steps 6), the light receptor albumen 4 is modified on 2 surface of the graphene, is based on
The bionical optical detector of graphene of thermoregulation energy.Wavelength selectivity is realized using light receptor albumen, improves absorptivity, and
And the optical sensor prepared using light receptor albumen will have the structure more simpler than conventional photodetectors, less expensive system
Cause this and higher sensitivity.
Embodiment two
Fig. 2 l are please referred to, it is described the present invention also provides a kind of bionical optical detector of graphene based on thermoregulation energy
The bionical optical detector of graphene based on thermoregulation energy is prepared using the preparation method in one scheme of embodiment, institute
Stating the bionical optical detector of graphene based on thermoregulation energy includes:Micro-heater platform 1;Graphene 2, be located at it is described it is micro- plus
On hot device platform 1;Active film (not shown) is formed in the surface of the graphene 2;Light receptor albumen 4 is formed in institute
It states on active film.
As an example, the micro-heater platform 1 includes successively from bottom to top:
Substrate 11, including a heat-insulation chamber 17;
Composite membrane 12 is located at 17 top of the heat-insulation chamber, including heating film region and supporting beam area, the supporting beam area connect
Connect the heating film region and the substrate 11;
Resistance device 130, including resistive heater 131, first is for electrical lead 132, the first current electrode 133, wherein extremely
Few resistive heater 131 is formed on the heating film region;
Insulating layer 14, is formed on the resistance device 130, at least covers the resistive heater 131;
Electrode device 150 is formed on the insulating layer 14, and include test electrode 151, second for electrical lead 152,
Second current electrode 153, wherein at least described test electrode 151 is correspondingly arranged with the resistive heater 131, the graphite
Alkene 2 at least covers the test electrode 151.
Preferably, the composite membrane 12 is the composite membrane that at least one layer of silicon oxide film and at least one layer of silicon nitride film are formed.
It is further preferred that the composite membrane 12 is, being sequentially depositing a layer thickness first with low-pressure chemical vapor deposition (LPCVD) is
The silica and a layer thickness of 0.1 μm~0.5 μm (the present embodiment is 0.2 μm) are 0.1 μm~0.5 μm, and (the present embodiment is 0.2 μ
M) silicon nitride;And then using plasma enhanced chemical vapor deposition (PECVD) be sequentially depositing a layer thickness be 0.1 μm~
The silica of 0.5 μm (the present embodiment is 0.2 μm) and the nitridation that a layer thickness is 0.1 μm~0.5 μm (the present embodiment is 0.2 μm)
Silicon.Further, if the composite membrane is formed by two layers or more silicon oxide film and two layers or more silicon nitride film, the preferably described oxygen
SiClx film is alternately superimposed on the silicon nitride film.
Specifically, 150 thickness of the electrode device is 30nm~300nm, and in the present embodiment, the electrode device 150
Thickness be preferably 100nm.The thickness of the silicon nitride dielectric layer is 400nm~600nm, in the present embodiment, preferably
500nm。
As an example, the test electrode 151 is interdigital electrode.
Specifically, the test electrode 151 is interdigital electrode, wherein build built in field using interdigital electrode, more effectively
Driving photo-generated carrier flowing so that response signal enhance, it is of course also possible to for other shapes electrode, such as it is snakelike
Electrode etc., this is not restricted.
As an example, the active film be active group 3 active film, the light receptor albumen 4 with it is described
The active group 3 of active film combines and forms covalent bond, to connect the light receptor albumen 4 and the active film.
Specifically, the active film is ending with the active group, in order to connect the light receptor albumen 4, institute
The combination that active group is one or more of amino active group, carboxyl-reactive group, aldehyde radical active group is stated,
In other embodiment, or can realize thin with the same or analogous activity with other active groups of this step function
Film.
Specifically, modifying the light receptor albumen 4 on 2 surface of the graphene, obtain based on thermoregulation energy
The bionical optical detector of graphene.Wavelength selectivity is realized using light receptor albumen, improves absorptivity, and use light receptor egg
The optical sensor prepared in vain will have the structure more simpler than conventional photodetectors, less expensive manufacturing cost and higher
Sensitivity.
In conclusion the present invention provide it is a kind of based on thermoregulation can the bionical optical detector of graphene and its preparation side
Method, the preparation method include the following steps:1) graphene and micro-heater platform are provided, and the graphene is transferred to institute
It states on micro-heater platform;2) structure that step 1) obtains is placed in chemical vapour deposition reactor furnace and is annealed;3) using examination
The graphene surface after annealing is modified in agent, thin with the activity for forming active group in the graphene surface
Film;4) light receptor albumen, the active group of the light receptor albumen and the active film are formed in the active film surface
In conjunction with covalent bond is formed, to connect the light receptor albumen and the active film.Based on said program, the present invention by using
The heating structure of outstanding membrane type connects graphene, and modifies light receptor albumen on the surface of graphene, on the one hand uses light receptor albumen
It realizes wavelength selectivity, improves absorptivity;On the other hand using membrane type heating structure is hanged, substrate is reduced to graphene performance
It influences, more operating temperature can be adjusted by heating voltage, to adjust photo-generated carrier mobility and concentration, to improve light
The performance of sensitive detection parts.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology can all carry out modifications and changes to above-described embodiment without violating the spirit and scope of the present invention.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should by the present invention claim be covered.
Claims (17)
1. a kind of preparation method of the bionical optical detector of graphene based on thermoregulation energy, which is characterized in that including as follows
Step:
1) graphene and micro-heater platform are provided, and the graphene is transferred on the micro-heater platform;
2) structure that step 1) obtains is placed in chemical vapour deposition reactor furnace and is annealed;
3) graphene surface after annealing is modified using reagent, it is active to be formed in the graphene surface
The active film of group;
4) light receptor albumen, the active group of the light receptor albumen and the active film are formed in the active film surface
In conjunction with covalent bond is formed, to connect the light receptor albumen and the active film.
2. the preparation method of the graphene bionical optical detector according to claim 1 based on thermoregulation energy, special
Sign is, in step 1), the micro-heater platform is made of following steps:
A substrate 1-1) is provided, and in forming composite membrane on the substrate, the composite membrane is for defining heating film region and branch
The areas Cheng Liang;
1-2) in formation heating metal layer on the composite membrane, and by the heating metallic layer graphic to obtain resistance device,
The resistance device includes resistive heater, first for electrical lead, the first current electrode, and at least described resistive heater is located at institute
State heating film region;
1-3) in forming insulating layer on the heating metal layer;
1-4) in formation test metal layer on the insulating layer, and by the test metallic layer graphic to obtain electrode device,
The electrode device includes test electrode, second for electrical lead, the second current electrode, at least described test electrode and the heating
Resistance wire is correspondingly arranged up and down, in addition, the graphene at least covers the test electrode;
1-5) in step 1-4) film release window is formed in the structure that is formed, and expose the substrate;
1-6) by described in the film release window erodable section substrate formed heat-insulation chamber, with release the heating film region and
Supporting beam area.
3. the preparation method of the graphene bionical optical detector according to claim 2 based on thermoregulation energy, special
Sign is, step 1-1) in, the substrate is the silicon substrate in (100) face, and the composite membrane is at least one layer of silicon oxide film and extremely
The composite membrane that few one layer of silicon nitride film is formed.
4. the preparation method of the graphene bionical optical detector according to claim 2 based on thermoregulation energy, special
Sign is, step 1-4) in, the test electrode is interdigital electrode.
5. the preparation method of the graphene bionical optical detector according to claim 2 based on thermoregulation energy, special
Sign is, step 1-6) in, the shape in the supporting beam area is linear or snakelike.
6. the preparation method of the graphene bionical optical detector according to claim 1 based on thermoregulation energy, special
Sign is, in step 1), the graphene is transferred on the micro-heater platform using direct transfer process or PMMA methods.
7. the preparation method of the graphene bionical optical detector according to claim 1 based on thermoregulation energy, special
Sign is that step 2) specifically includes:
2-1) inert gas is used to carry out ventilation and gas exhaust treatment to the reacting furnace;
2-2) inert gas is passed through into the reacting furnace at a temperature of first;
2-3) inert gas and hydrogen are passed through into the reacting furnace simultaneously under second temperature;
The flow of the inert gas and the hydrogen 2-4) is reduced, and is cooled down to the reacting furnace.
8. the preparation method of the graphene bionical optical detector according to claim 7 based on thermoregulation energy, special
Sign is, step 2-1) in, the flow of the inert gas is 500sccm~2000sccm, when the ventilation and gas exhaust treatment
Between be 2min~3min.
9. the preparation method of the graphene bionical optical detector according to claim 7 based on thermoregulation energy, special
Sign is, step 2-2) in, first temperature is 200 DEG C~300 DEG C, the flow of the inert gas be 500sccm~
2000sccm。
10. the preparation method of the graphene bionical optical detector according to claim 7 based on thermoregulation energy, special
Sign is, step 2-3) in, the second temperature is 300 DEG C~400 DEG C, and keep under the second temperature 5min~
10min, total flow 500sccm~2000sccm of the hydrogen being passed through after heat preservation and the mixed gas of the inert gas,
The volume fraction of hydrogen described in the mixed gas is 30%~50%, is passed through the time of the inert gas and the hydrogen
For 40min~120min.
11. the preparation method of the graphene bionical optical detector according to claim 7 based on thermoregulation energy, special
Sign is, step 2-4) in, flow 50sccm~200sccm of the inert gas, the flow 10sccm of the hydrogen~
The mode of 40sccm, the cooling are reacting furnace Temperature fall.
12. the preparation method of the graphene bionical optical detector according to claim 1 based on thermoregulation energy, special
Sign is, in step 3), the reagent includes 1,5-diaminonaphthalene, 1- pyrenes butyric acid, glutaraldehyde, 1- (3- dimethylamino-propyls)-
The combination of one or more of 3- ethyl-carbodiimide hydrochlorides and n-hydroxysuccinimide;The active group is
The combination of one or more of amino active group, carboxyl-reactive group, aldehyde radical active group.
13. the preparation method of the graphene bionical optical detector according to claim 1 based on thermoregulation energy, special
Sign is, in step 4), the light receptor albumen include opsin class, phytochrome class, cryptochrome class, to photopigment class,
The combination of one or more of BLUF structural domains class, ultraviolet light receptor class.
14. a kind of bionical optical detector of graphene based on thermoregulation energy, which is characterized in that including:
Micro-heater platform;
Graphene is located on the micro-heater platform;
Active film is formed in the surface of the graphene;
Light receptor albumen is formed on the active film.
15. the graphene bionical optical detector according to claim 14 based on thermoregulation energy, which is characterized in that institute
Stating micro-heater platform includes successively from bottom to top:
Substrate, including a heat-insulation chamber;
Composite membrane is located above the heat-insulation chamber, including heating film region and supporting beam area, and the supporting beam area connection is described to be added
Hotting mask area and the substrate;
Resistance device, including resistive heater, first are for electrical lead, the first current electrode, wherein at least described resistive heater
It is formed on the heating film region;
Insulating layer, is formed on the resistance device, at least covers the resistive heater;
Electrode device is formed on the insulating layer, and includes test electrode, second for electrical lead, the second current electrode,
In, at least described test electrode is correspondingly arranged up and down with the resistive heater, and the graphene at least covers the test electricity
Pole.
16. the graphene bionical optical detector according to claim 15 based on thermoregulation energy, which is characterized in that institute
It is interdigital electrode to state test electrode.
17. the graphene bionical optical detector according to claim 14 based on thermoregulation energy, which is characterized in that institute
The active film that active film is active group is stated, the light receptor albumen is combined with the active group of the active film
Covalent bond is formed, to connect the light receptor albumen and the active film.
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