CN106198674B - A kind of mesoporous graphene preparation process and it is based on mesoporous graphene field effect transistor biosensor - Google Patents
A kind of mesoporous graphene preparation process and it is based on mesoporous graphene field effect transistor biosensor Download PDFInfo
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- CN106198674B CN106198674B CN201610725988.7A CN201610725988A CN106198674B CN 106198674 B CN106198674 B CN 106198674B CN 201610725988 A CN201610725988 A CN 201610725988A CN 106198674 B CN106198674 B CN 106198674B
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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 process and it is based on mesoporous graphene field effect transistor biosensor, the nanosphere array of assembling cycle arrangement on the surface of graphene, deposited metal film, remove nanosphere, as exposure mask, the mesoporous graphene for preparing different pore size obtains the mesoporous graphene of different pitchs of holes, achievees the purpose that regulate and control graphene energy gap；With the active oxygen-containing group that oxygen plasma etch graphene is formed, bioactive molecule can connect；The use for avoiding the common bridging agents such as AuNPs, glutaraldehyde, pyrene butyric acid, 1- hydroxysuccinimide eater -1- pyrene butyric acid, greatly reduces the manufacturing cost of biosensor；Mesoporous graphene field effect transistor biosensor opens the with gap of graphene, has biggish current on/off ratio, and minimal amount of biomolecule can make the conductivity of graphene conductive channel generate significant response, greatly improve the sensitivity of detection.
Description
Technical field
The invention belongs to field of biosensors, in particular to a kind of mesoporous graphene preparation process and be based on mesoporous graphene
Field effect transistor biosensor.
Background technique
Graphene is a kind of novel two-dimentional carbon material, shows excellent electrical properties, the nanometer electricity based on graphene
Sub- device is considered as the excellent substitute of conventional semiconductors, and still, zero band gap of intrinsic graphene is to limit it deeply to apply
An important factor for, the semiconductor material of non-zero band gap is needed if field effect transistor；Therefore, regulation graphene band gap width tool
It is significant.
With the development of graphene preparation technology, the graphene for obtaining structural integrity is comparatively easy, but graphene
Band gap width is almost nil or very little, be used to prepare semiconductor devices and be extremely restricted；Currently, regulation graphene band gap is wide
Degree has following several method:
(1) physical method；Physical method carries out the regulation of graphene band gap width mainly for graphene geometric dimension etc.；Be compared with
Commonly to regulate and control graphene band gap width method, regulate and control band gap width especially by the geometric dimension effect of graphene,
Studies have shown that the graphene nanobelt that unidimensional scale is limited has certain band gap；Currently, graphene alkene nanobelt is prepared, it is main
There is etching method and cut carbon nanotube method, the former mainly utilizes etching method, such as photoengraving, electron beam lithography, focused ion
Flake graphite alkene is carved into quasi-one-dimensional graphene nanobelt by beam photoetching etc.；The latter is mainly the potassium permanganate for using strong oxidizing property
Carbon nanotube cutting is opened with sulfuric acid, plasma etching, electrochemical method etc., forms graphene nanobelt；It can also be in graphite
Alkene on piece, formation is mesoporous, is graphene nanobelt between hole, keeps graphene unidimensional scale limited, to open band gap；In addition, sharp
It can also lead to the generation of graphene band gap to the influence of graphene with substrate；
(2) chemical doping method；Chemical doping method is divided into impurity and adsorption doping；Graphene passes through chemical gaseous phase
Deposition method can be prepared with large area, during the preparation process or in post-processing, by introducing different reaction sources, can make stone
Part carbon atom in black alkene 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 certain fields, need to develop prepare it is high-quality
Measure the preparation process of few layer and multi-layer graphene；For example, the native band gap of single-layer graphene is zero, have very in semiconductor field
Big application limitation；Existing research shows that the bilayer graphene of AB stacking provisions can be one under the action of extra electric field
Determine to generate continuously adjustable band gap in range, although numerous studies have been done for Growing Double-Layer graphene, due to growth
Bilayer graphene can not accuracy controlling, or uneven for random layer stacking provisions or the number of plies, there are more three layers or single layer regions；
How controlling stacking provisions, improving number of plies homogeneity is that current CVD growth is double-deck and multi-layer graphene studies the common difficulty faced
Topic.
In conclusion designing the geometric dimension of graphene by physical method to regulate and control with gap, simple possible；But due to
The restriction of photoetching technique, etching method prepare the width of graphene nanobelt, are extremely limited.In addition, carbon nanotube is cut,
The homogeneity that not can guarantee graphene nanobelt, is also unsuitable for large scale preparation；Being formed on graphene mesoporous is to carry out band gap
The feasible program of regulation can regulate and control the energy gap of graphene by the size of mesoporous pore size；201210032772.4 benefit of patent
With anodised aluminium (AAO) template, graphene nano hole array is prepared, but AAO template making technique is complex, including high-purity
The techniques such as aluminium pre-treatment, once oxidation, secondary oxidation, through-hole need for the pore size and pitch of holes difference for guaranteeing AAO template
Control Arrays Aluminum Films in Acid Solution, concentration, temperature, oxidizing potential and time etc.；Relative to AAO template, soft template is generally all held very much
Easily construct, it is easy to operate without complicated equipment, it is low in cost etc., cause the extensive concern of people；California, USA university Lip river China fir
The section edge cutting edge of a knife or a sword in rock branch school etc. has prepared mesoporous graphene, has successfully opened the with of graphene by block polymer soft template
Gap, and can achieve the purpose that regulate and control graphene with gap by adjusting pitch of holes；It is well known that graphene has huge ratio
Block polymer soft template is covered on graphene by surface area, will increase graphene surface cleaning difficulty, graphene surface meeting
The problems such as having polymer residue, influencing field-effect transistor performance.
Summary of the invention
The technical problems to be solved by the invention are to provide a kind of mesoporous graphene preparation work for above-mentioned state of the art
Skill and be based on mesoporous graphene field effect transistor biosensor, by open graphene energy gap, be prepared for a kind of mesoporous stone
Black alkene, and a kind of field effect transistor biosensor is prepared for this, current on/off ratio with higher can be effectively to super
The biomolecule of low content is detected.
In order to solve the above technical problems, a kind of technical solution that the present invention takes is:
A kind of mesoporous graphene preparation process, comprises the following steps that:
(1) graphene film is prepared in substrate；
(2) in the nanosphere array of graphene film over-assemble periodic arrangement；By Si/SiO2/ graphene film/it receives
Rice micro-sphere array, high-temperature heating make nanosphere body and graphene close adhesion；
(3) in Si/SiO2Metal film on/graphene film/nanosphere array is removed with organic solvent and is polymerize
Object nanosphere；
(4) graphene is etched using oxygen plasma etching body, then etches away metal and forms mesoporous graphene；
(5) when oxygen plasma etch graphene, oxygen-containing group is formed in graphene edge, oxygen-containing group is changed into-
COOH connects biological identification molecule；
(4) on mesoporous graphene, field effect transistor is made；Made with Ag/AgCl or platinum filament insertion fluid to be measured sample
For reference electrode；Source, drain electrode are metal electrode.
Preferably, in the step (1) graphene film be CVD method synthesis graphene or redox graphene or machine
Tool removes graphene.
Preferably, metallic film is Al metallic film or Cu metallic film or Ni metallic film in the step (3).
Preferably, oxygen-containing group is hydroxyl or epoxy group or carboxyl or carbonyl in the step (5).
Another technical solution adopted by the present invention to solve the technical problem thereof is that:
One kind being based on mesoporous graphene field effect transistor biosensor, including basal layer, is set on the basal layer
Mesoporous graphene layer, one group of drain-source electrodes is equipped at intervals on the mesoporous graphene layer, between one group of drain-source electrodes
Mesoporous graphene layer is equipped with bio-identification layer, and the top of the bio-identification layer is equipped with reference electrode, one group of leakage, source electricity
One is formed between pole and the bio-identification layer for conductive conducting channel, in the reference electrode and the conducting channel
The connection of sample solution plug-in type.
Preferably, the basal layer is Si/SiO2Basal layer.
Preferably, the mesoporous graphene layer is equipped with the mesoporous of multiple uniform intervals arrangement.
Preferably, the source, electric leakage extremely 5-10nmCr and 30-50nmAu are constituted.
Preferably, a length of 10-20 μm of the conducting channel, width are 20-30 μm.
The positive effect of the present invention is shown: the present invention provides a kind of mesoporous graphene preparation process and based on mesoporous graphite
Alkene field effect transistor biosensor；On the surface of graphene assembling cycle arrangement nanosphere array, evaporating Al, Cu,
Ni etc., removal nanosphere prepare the mesoporous graphene of different pore size, obtain the mesoporous of different pitchs of holes as exposure mask
Graphene achievees the purpose that regulate and control graphene energy gap；It, can be with the active oxygen-containing group that oxygen plasma etch graphene is formed
Connect bioactive molecule；Avoid the common companies such as AuNPs, glutaraldehyde, pyrene butyric acid, 1- hydroxysuccinimide eater -1- pyrene butyric acid
The use for connecing agent greatly reduces the manufacturing cost of biosensor；Mesoporous graphene field effect transistor biosensor,
The with gap of graphene is opened, there is biggish current on/off ratio, minimal amount of biomolecule can make graphene conductive ditch
The conductivity in road generates significant response, greatly improves the sensitivity of detection.
Detailed description of the invention
Attached drawing 1 is graphene film structural schematic diagram；
Attached drawing 2 is the structural schematic diagram after the nanosphere array of graphene film over-assemble periodic arrangement；
Attached drawing 3 is in si/sio2Structural schematic diagram after metal film on/graphene film/nanosphere array；
Attached drawing 4 is that organic solvent removes structural schematic diagram after polymer nanocomposite ball；
Attached drawing 5 is mesoporous graphene-structured schematic diagram；
Attached drawing 6 is based on mesoporous graphene field effect transistor biosensor structure schematic diagram；
The test of 7 detection device of attached drawing is based on mesoporous graphene field effect transistor biosensor result schematic diagram.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out under the premise of the technical scheme of the present invention
Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment is as follows:
(1) graphene film 11 is transferred to Si/SiO such as attached drawing 1 by process for preparing graphenes by chemical vapour deposition film 112
In substrate 21, Si/SiO is obtained2/ graphene 22, cleans up, N2Drying is stand-by；
(2) the PMMA nanosphere 23 that partial size is 8-80nm is dispersed in deionized water/dehydrated alcohol (volume ratio of 5-10mL
23 dispersion liquid of PMMA nanosphere is slowly added dropwise in the surfactant SDS solution of 0.5-5wt% in the mixed solvent 1:1),
PMMA nanosphere 23 assembles to form single layer nanosphere film, Si/SiO in air liquid interface222 oblique cutting of/graphene enter liquid level hereinafter,
On the surface of graphene by the transfer of 23 film of single layer PMMA nanosphere；
(3) Si/SiO for obtaining (2)2/ graphene/PMMA nanosphere, 120-150 DEG C of baking 10-30min, makes PMMA
Nanosphere 23 is closely attached to 22 surface of graphene, such as attached drawing 2；Then, in the metallic film 31 of its surface vapor deposition 10-100nm, such as
Metal Al film, such as attached drawing 3；
(4) (3) are impregnated in acetone, structure is 41 after removing PMMA nanosphere 23, such as attached drawing 4；Successively with anhydrous second
Alcohol, deionized water clean up, and N2 drying etches graphene with oxygen plasma；Remove Al with the hydrochloric acid of 0.5mol/L, go from
Sub- water repeated flushing, N2It dries up to get Si/SiO is arrived2/ mesoporous graphene 51；Such as attached drawing 5；
(5) micro-nano technology technique is used, production is the field effect transistor of conducting channel with mesoporous graphene 51；Including base
Bottom 61, the mesoporous graphene layer 62 on basal layer 61, be equipped at intervals on mesoporous graphene layer 62 one group of source electrode 63,
Drain electrode 64, the mesoporous graphene layer 62 between one group of source electrode 63, drain electrode 64 are equipped with bio-identification layer 65, and biology is known
The top of other layer 65 is equipped with reference electrode 66, forms one between one group of source electrode 63, drain electrode 64 and bio-identification layer 65 and is used for
Conductive conducting channel, reference electrode are connect with the sample solution plug-in type in conducting channel；Wherein source electrode, drain electrode
It is constituted for 5-10nmCr and 30-50nmAu, a length of 10-20 μm of conducting channel, width is 20-30 μm, using liquid grid technique, by Ag/
AgCl electrode, which is inserted into sample solution, is used as reference electrode；Such as attached drawing 6；
(6) when oxygen plasma etch graphene, oxygen-containing group (such as hydroxyl, epoxy group, carboxylic are formed in graphene edge
Base, carbonyl etc.), carboxylated reagent (monoxone containing 50-200mmol/L, the sodium hydroxide solution of 100-500mmol/L) is covered
It covers on mesoporous graphene, is incubated at room temperature 2-4h, first rinsed with 0.1-0.5mmol/L hydrochloric acid, then rushed repeatedly with deionized water
It washes, oxygen-containing group is made to be changed into-COOH, vacuum drying oven drying, and with NHS/EDC activation-COOH；With 0.1 × PBS of pH=7.4
Buffer solution is solvent, and compound concentration is the PSA(prostate specific antigen of 10-30 μ g/mL) antibody-solutions, 2- is stood at room temperature
After 5h, rinsed well with 0.1 × PBS solution of pH=7.4, deionized water；
(7) device for obtaining (6) is placed in 1-2h in the ethanolamine solutions of 50-100mM at room temperature, prevents non-specificity
Absorption；It is then that 0.05%, Tween20 closes not connected bio-identification with 0.1 × PBST(Tween20 volume fraction of pH=7.4
The graphene of molecule) solution rinses well, N2Drying, the PSA of compound concentration 0,10,100,1000fg/mL, using independently grinding
The portable detection equipment of hair detects it, testing conditions VDS=1V, Vg=0.1V, test result are shown in attached drawing 7.
The present invention is described in detail above, its object is to allow the personage for being familiar with this field technology that can understand this
The content of invention is simultaneously implemented, and it is not intended to limit the scope of the present invention, all Spirit Essence institutes according to the present invention
The equivalent change or modification of work, should be covered by the scope of protection of the present invention.
Claims (4)
1. a kind of mesoporous graphene preparation process, which is characterized in that comprise the following steps that:
(1) graphene film is prepared in substrate；
(2) in the nanosphere array of graphene film over-assemble periodic arrangement；By Si/SiO2/ graphene film/nanometer is micro-
Ball array, high-temperature heating, makes nanosphere body and graphene close adhesion；
(3) in Si/SiO2Metal film on/graphene film/nanosphere array removes polymer nano with organic solvent
Rice ball；
(4) graphene is etched using oxygen plasma etching body, then etches away metal and forms mesoporous graphene；
(5) when oxygen plasma etch graphene, oxygen-containing group is formed in graphene edge, oxygen-containing group is changed into-COOH,
Connect biological identification molecule；
(6) on mesoporous graphene, field effect transistor is made；Fluid to be measured sample is inserted into as ginseng using Ag/AgCl or platinum filament
Compare electrode；Source, drain electrode are metal electrode.
2. a kind of mesoporous graphene preparation process according to claim 1, which is characterized in that graphite in the step (1)
Alkene film is the graphene that CVD method synthesizes or redox graphene or mechanical stripping graphene.
3. a kind of mesoporous graphene preparation process according to claim 1, which is characterized in that metal in the step (3)
Film is Al metallic film or Cu metallic film or Ni metallic film.
4. a kind of mesoporous graphene preparation process according to claim 1, which is characterized in that oxygen-containing in the step (5)
Group is hydroxyl or epoxy group or carboxyl or carbonyl.
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