CN106198674A - A kind of mesoporous Graphene preparation technology and based on mesoporous graphene field effect transistor biosensor - Google Patents
A kind of mesoporous Graphene preparation technology and based on mesoporous graphene field effect transistor biosensor Download PDFInfo
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- CN106198674A CN106198674A CN201610725988.7A CN201610725988A CN106198674A CN 106198674 A CN106198674 A CN 106198674A CN 201610725988 A CN201610725988 A CN 201610725988A CN 106198674 A CN106198674 A CN 106198674A
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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
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
- G01N27/3275—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction
- G01N27/3278—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction involving nanosized elements, e.g. nanogaps or nanoparticles
Abstract
The present invention relates to a kind of mesoporous Graphene preparation technology and based on mesoporous graphene field effect transistor biosensor, Nano microsphere array in the arrangement of graphenic surface assembling cycle, deposited metal film, remove Nano microsphere, as mask, prepare the mesoporous Graphene of different pore size, obtain the mesoporous Graphene of different pitch of holes, reach the purpose of Graphene energy gap；The active oxy radical formed with oxygen plasma etch Graphene, can connect bioactive molecule；Avoid the use of the conventional bridging agents such as AuNPs, glutaraldehyde, pyrene butanoic acid, 1 hydroxysuccinimide eater 1 pyrene butanoic acid, greatly reduce the manufacturing cost of biosensor；Mesoporous graphene field effect transistor biosensor, opens the gap of Graphene, has bigger current on/off ratio, and minimal amount of biomolecule can make the electrical conductivity of graphene conductive raceway groove produce significantly response, is greatly improved the sensitivity of detection.
Description
Technical field
The invention belongs to field of biosensors, particularly to a kind of mesoporous Graphene preparation technology and based on mesoporous Graphene
Field-effect transistor biosensor.
Background technology
Graphene is a kind of novel Two-dimensional Carbon material, shows excellent electrical properties, nanoelectronic device based on Graphene
Part is considered as the excellent substitute of conventional semiconductors, but, zero band gap of intrinsic Graphene is to limit its weight deeply applied
Want factor, as field-effect transistor is accomplished by the semi-conducting material of non-zero band gap；Therefore, regulation and control Graphene band gap width has weight
Want meaning.
Along with the development of graphene preparation technology, the Graphene obtaining structural integrity is comparatively easy, but Graphene
Band gap width almost nil or the least, be used for preparing semiconductor device and be extremely restricted；At present, regulation and control graphene ribbon gap length
Spend and have following several method:
(1) Physical；Physical carries out the regulation and control of Graphene band gap width mainly for Graphene physical dimension etc.；It is the most normal
Regulation and control Graphene band gap width method, the physical dimension effect especially by Graphene regulates and controls band gap width, research
Showing, the limited graphene nanobelt of unidimensional scale has certain band gap；At present, prepare Graphene alkene nano belt, mainly have
Etching method and cutting CNT method, the former is mainly by etching method, such as photoengraving, beamwriter lithography, focused ion Shu Guang
Carve, flake graphite alkene is carved into quasi-one-dimensional graphene nanobelt；The latter is mainly with potassium permanganate and the sulfur of strong oxidizing property
CNT cutting is opened by acid, plasma etching, electrochemical method etc., forms graphene nanobelt；Can also be at graphene film
On, formed mesoporous, be graphene nanobelt between hole, make Graphene unidimensional scale limited, thus open band gap；Additionally, utilize base
The end, can also cause the generation of Graphene band gap to the impact of Graphene；
(2) chemical doping method；Chemical doping method is divided into impurity and surface adsorption doping；Graphene is deposited by chemical gaseous phase
Method can be prepared with large area, in preparation process or in post processing, by introducing different reaction sources, can make Graphene
Part carbon atom in lattice structure is replaced by other atoms, forms impurity；
(3) number of plies control methods；Single-layer graphene is difficult to meet the application requirement in some field, needs development to prepare high-quality few
Layer and the preparation technology of multi-layer graphene；Such as, the native band gap of single-layer graphene is zero, has the biggest at semiconductor applications
Application limitation；There are some researches show, the bilayer graphene of AB stacking provisions can be at certain model under the effect of extra electric field
Enclose the continuously adjustable band gap of interior generation, although numerous studies have been done for Growing Double-Layer Graphene, but due to the bilayer of growth
Graphene cannot accuracy controlling, or be random layer stacking provisions, or the number of plies be uneven, there is more three layer or monolayer region；How
Control stacking provisions, raising number of plies homogeneity is that current CVD growth is double-deck and multi-layer graphene studies the common difficulty faced.
In sum, by Physical, the physical dimension of design Graphene regulates and controls gap, simple possible；But, due to
The restriction of photoetching technique, etching method is prepared the width of graphene nanobelt, is extremely limited.It addition, cutting CNT,
The homogeneity of graphene nanobelt cannot be ensured, be also unsuitable for preparing on a large scale；Graphene is formed and mesoporous is by band gap
The feasible program of regulation and control, can regulate and control the energy gap of Graphene by the size of mesoporous pore size；Patent 201210032772.4 profit
By anodised aluminium (AAO) template, prepare grapheme nano-pore array, but AAO template making technique is complex, including high-purity
The techniques such as aluminum pre-treatment, once oxidation, secondary oxidation, through hole, different with pitch of holes for ensureing the pore size of AAO template, need
Arrays Aluminum Films in Acid Solution to be controlled, concentration, temperature, oxidizing potential and time etc.；Relative to AAO template, soft template is held the most very much
Easily construct, it is not necessary to complicated equipment, easy to operate, with low cost etc., cause the extensive concern of people；California, USA university Lip river China fir
The section edge cutting edges of a knife or a sword in rock branch school etc., by block polymer soft template, have been prepared mesoporous Graphene, have successfully been opened Graphene
Gap, and can reach by adjustment hole spacing the purpose of Graphene gap；It is known that Graphene has huge ratio
Surface area, covers block polymer soft template on Graphene, can increase graphenic surface cleaning difficulty, graphenic surface meeting
There is polymer residue, affect the problems such as field-effect transistor performance.
Summary of the invention
Invent and to be solved technical problem is that for above-mentioned prior art present situation, it is provided that a kind of mesoporous Graphene prepares work
Skill and based on mesoporous graphene field effect transistor biosensor, by opening Graphene energy gap, is prepared for a kind of mesoporous stone
Ink alkene, and it is prepared for a kind of field-effect transistor biosensor with this, there is higher current on/off ratio, can be effectively to super
The biomolecule of low content detects.
For solving above technical problem, a kind of technical scheme that the present invention takes is:
A kind of mesoporous Graphene preparation technology, comprises the following steps that:
(1) in substrate, graphene film is prepared；
(2) the Nano microsphere array of assembling cycle arrangement on graphene film；By Si/SiO2/ graphene film/nanometer is micro-
Ball array, high-temperature heating, make nanosphere body and Graphene close adhesion；
(3) at Si/SiO2Metal film on/graphene film/Nano microsphere array, removes polymer nano with organic solvent
Rice ball；
(4) use oxygen plasma etching body etching Graphene, then etch away metal and form mesoporous Graphene；
(5), during oxygen plasma etch Graphene, form oxy radical in graphene edge, oxy radical be changed into-COOH,
Connect biological identification molecule；
(4) on mesoporous Graphene, fabricating yard effect transistor；Fluid to be measured sample is inserted as ginseng using Ag/AgCl or platinum filament
Compare electrode；Source, drain electrode are metal electrode.
Preferably, in described step (1), graphene film is Graphene or redox graphene or the machine of CVD synthesis
Graphene peeled off by tool.
Preferably, in described step (3), metallic film is Al metallic film or Cu metallic film or Ni metallic film.
Preferably, in described step (5), oxy radical is hydroxyl or epoxy radicals or carboxyl or carbonyl.
What the present invention solved that its technical problem used another solution is that
A kind of based on mesoporous graphene field effect transistor biosensor, including basal layer, it is located at Jie on described basal layer
Hole graphene layer, described mesoporous graphene layer is interval with one group of drain-source electrodes, mesoporous between described one group of drain-source electrodes
Graphene layer is provided with bio-identification layer, described bio-identification layer be arranged over reference electrode, described one group of leakage, source electrode and
Formed one for the conducting channel of conduction between described bio-identification layer, tested with in described conducting channel of described reference electrode
Sample solution plug-in type connects.
Preferably, described basal layer is Si/SiO2Basal layer.
Preferably, described mesoporous graphene layer is provided with the mesoporous of multiple uniform intervals arrangement.
Preferably, described source, extremely 5-10nmCr and 30-50nmAu that leak electricity are constituted.
Preferably, described conducting channel a length of 10-20 μm, a width of 20-30 μm.
The positive effect of the present invention shows: the present invention provides a kind of mesoporous Graphene preparation technology and based on mesoporous graphite
Alkene field-effect transistor biosensor；Graphenic surface assembling cycle arrangement Nano microsphere array, evaporating Al, Cu,
Ni etc., remove Nano microsphere, as mask, prepare the mesoporous Graphene of different pore size, obtain the mesoporous of different pitch of holes
Graphene, reaches the purpose of Graphene energy gap；The active oxy radical formed with oxygen plasma etch Graphene, permissible
Connect bioactive molecule；Avoid the conventional companies such as AuNPs, glutaraldehyde, pyrene butanoic acid, 1-hydroxysuccinimide eater-1-pyrene butanoic acid
Connect the use of agent, greatly reduce the manufacturing cost of biosensor；Mesoporous graphene field effect transistor biosensor,
Opening the gap of Graphene, have bigger current on/off ratio, minimal amount of biomolecule can make graphene conductive ditch
The electrical conductivity in road produces significantly response, is greatly improved the sensitivity of detection.
Accompanying drawing explanation
Accompanying drawing 1 is graphene film structural representation；
Accompanying drawing 2 is the structural representation on graphene film after the Nano microsphere array of assembling cycle arrangement；
Accompanying drawing 3 is at si/sio2Structural representation after metal film on/graphene film/Nano microsphere array；
Accompanying drawing 4 is structural representation after organic solvent removal polymer nanocomposite ball；
Accompanying drawing 5 is mesoporous graphene-structured schematic diagram；
Accompanying drawing 6 is based on mesoporous graphene field effect transistor biosensor structure schematic diagram；
Accompanying drawing 7 detects equipment and tests based on mesoporous graphene field effect transistor biosensor result schematic diagram.
Detailed description of the invention
Elaborating embodiments of the invention below, the present embodiment is carried out under premised on technical solution of the present invention
Implement, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following enforcement
Example.
Embodiment is as follows:
(1) process for preparing graphenes by chemical vapour deposition thin film 11, such as accompanying drawing 1, transfers to Si/SiO by graphene film 112Substrate
On 21, obtain Si/SiO2/ Graphene 22, cleans up, N2Dry up stand-by；
(2) the PMMA nanosphere 23 that particle diameter is 8-80nm is dispersed in the deionized water/dehydrated alcohol (volume ratio 1:1) of 5-10mL
Mixed solvent in, PMMA nanosphere 23 dispersion liquid is slowly added dropwise in the surfactant SDS solution of 0.5-5wt%, PMMA
Nanosphere 23 assembles in air liquid interface and forms monolayer nanosphere thin film, Si/SiO2/ Graphene 22 oblique cutting enters below liquid level, will be single
Layer PMMA nanosphere 23 thin film shifts at graphenic surface；
(3) Si/SiO that (2) are obtained2/ Graphene/PMMA nanosphere, 120-150 DEG C of baking 10-30min, make PMMA nanometer
Ball 23 is closely attached to Graphene 22 surface, such as accompanying drawing 2；Then, at the metallic film 31 of its surface evaporation 10-100nm, such as metal
Al thin film, such as accompanying drawing 3；
(4) (3) being soaked in acetone, after removing PMMA nanosphere 23, structure is 41, such as accompanying drawing 4；Successively with dehydrated alcohol, go
Ionized water cleans up, and N2 dries up, and etches Graphene by oxygen plasma；Al, deionized water is removed with the hydrochloric acid of 0.5mol/L
Repeatedly rinse, N2Dry up, i.e. obtain Si/SiO2/ mesoporous Graphene 51；Such as accompanying drawing 5；
(5) use micro-nano technology technique, make the field-effect transistor with mesoporous Graphene 51 as conducting channel；Including basal layer
61, the mesoporous graphene layer 62 being located on basal layer 61, mesoporous graphene layer 62 is interval with one group of source electrode 63, electric leakage
Pole 64, the mesoporous graphene layer 62 between a group of source electrode 63, drain electrode 64 is provided with bio-identification layer 65, bio-identification layer
65 be arranged over reference electrode 66, one group of source electrode 63, form one between drain electrode 64 and bio-identification layer 65 and be used for conducting electricity
Conducting channel, reference electrode is connected with the sample solution plug-in type in conducting channel；Wherein source electrode, leak electricity extremely 5-
10nmCr and 30-50nmAu is constituted, conducting channel a length of 10-20 μm, a width of 20-30 μm, uses liquid grid technique, by Ag/AgCl
Electrode inserts in sample solution as reference electrode；Such as accompanying drawing 6；
(6), during oxygen plasma etch Graphene, oxy radical is formed (such as hydroxyl, epoxy radicals, carboxyl, carbonyl in graphene edge
Base etc.), carboxylated reagent (monoxone containing 50-200mmol/L, the sodium hydroxide solution of 100-500mmol/L) is covered
On mesoporous Graphene, incubated at room 2-4h, first rinse with 0.1-0.5mmol/L hydrochloric acid, then repeatedly rinse with deionized water, make
Oxy radical is changed into-COOH, and vacuum drying oven is dried, and with NHS/EDC activation-COOH；Buffer with the 0.1 × PBS of pH=7.4
Solution is solvent, and compound concentration is the PSA(prostate specific antigen of 10-30 μ g/mL) antibody-solutions, left at room temperature 2-5h
After, clean with the 0.1 × PBS solution of pH=7.4, deionized water rinsing；
(7) device (6) obtained, is placed in 1-2h in the ethanolamine solutions of 50-100mM, prevents non-specific adsorption under room temperature；
Being 0.05% by 0.1 × PBST(Tween20 volume fraction of pH=7.4 subsequently, Tween20 closes and is not connected with biological identification molecule
Graphene) solution rinses well, N2Drying up, compound concentration is the PSA of 0,10,100,1000fg/mL, uses independent research
It is detected by portable detection equipment, and testing conditions is VDS=1V, Vg=0.1V, test result is shown in accompanying drawing 7.
Above the present invention is described in detail, its object is to allow the personage being familiar with this art will appreciate that this
Invention content and be carried out, can not limit the scope of the invention with this, all spirit institutes according to the present invention
The equivalence change made or modification, all should contain within the scope of the present invention.
Claims (9)
1. a mesoporous Graphene preparation technology, it is characterised in that comprise the following steps that:
(1) in substrate, graphene film is prepared；
(2) the Nano microsphere array of assembling cycle arrangement on graphene film；By Si/SiO2/ graphene film/nanometer is micro-
Ball array, high-temperature heating, make nanosphere body and Graphene close adhesion；
(3) at Si/SiO2Metal film on/graphene film/Nano microsphere array, removes polymer nano with organic solvent
Rice ball；
(4) use oxygen plasma etching body etching Graphene, then etch away metal and form mesoporous Graphene；
(5), during oxygen plasma etch Graphene, form oxy radical in graphene edge, oxy radical be changed into-COOH,
Connect biological identification molecule；
(6) on mesoporous Graphene, fabricating yard effect transistor；Fluid to be measured sample is inserted as ginseng using Ag/AgCl or platinum filament
Compare electrode；Source, drain electrode are metal electrode.
One the most according to claim 1 mesoporous Graphene preparation technology, it is characterised in that graphite in described step (1)
Alkene thin film is Graphene or redox graphene or the mechanical stripping Graphene of CVD synthesis.
One the most according to claim 1 mesoporous Graphene preparation technology, it is characterised in that metal in described step (3)
Thin film is Al metallic film or Cu metallic film or Ni metallic film.
One the most according to claim 1 mesoporous Graphene preparation technology, it is characterised in that oxygen-containing in described step (5)
Group is hydroxyl or epoxy radicals or carboxyl or carbonyl.
5. one kind based on mesoporous graphene field effect transistor biosensor, it is characterised in that include basal layer, is located at described
Mesoporous graphene layer on basal layer, described mesoporous graphene layer is interval with one group of source, drain electrode, described one group of source, leakage
Mesoporous graphene layer between electrode is provided with bio-identification layer, described bio-identification layer be arranged over reference electrode, described
One group of source, being formed one for the conducting channel of conduction between drain electrode and described bio-identification layer, described reference electrode is with described
Sample solution plug-in type in conducting channel connects.
One the most according to claim 5 is based on mesoporous graphene field effect transistor biosensor, it is characterised in that
Described basal layer is Si/SiO2Basal layer.
One the most according to claim 5 is based on mesoporous graphene field effect transistor biosensor, it is characterised in that
Described mesoporous graphene layer is provided with the mesoporous of multiple uniform intervals arrangement.
One the most according to claim 5 is based on mesoporous graphene field effect transistor biosensor, it is characterised in that
Described one group of source, extremely 5-10nmCr and 30-50nmAu that leak electricity are constituted.
One the most according to claim 5 is based on mesoporous graphene field effect transistor biosensor, it is characterised in that
Described conducting channel a length of 10-20 μm, a width of 20-30 μm.
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