CN106383196B - The biology sensor and preparation method of a kind of graphene/copper particle mixed structure - Google Patents
The biology sensor and preparation method of a kind of graphene/copper particle mixed structure Download PDFInfo
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- CN106383196B CN106383196B CN201610929042.2A CN201610929042A CN106383196B CN 106383196 B CN106383196 B CN 106383196B CN 201610929042 A CN201610929042 A CN 201610929042A CN 106383196 B CN106383196 B CN 106383196B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
- G01N30/92—Construction of the plate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
- G01N30/94—Development
Abstract
The invention discloses the biology sensor and preparation method of a kind of graphene/copper particle mixed structure, and the biology sensor, the layer structure that two-dimensional graphene is mixed with copper nano particles is attached with the upper surface of all-glass paper.Its preparation method be using Vacuum Coating method on all-glass paper copper plating film; the graphene of generation is set to be deposited on the copper film using chemical vapour deposition technique; copper film is set to be processed into copper nano particles layer at the same time, so that copper film forms the layer structure that two-dimensional graphene is mixed with copper nano particles.
Description
Technical field
The invention belongs to new material technology field, is related to a kind of biology sensor and its system of separable mixed biologic molecule
A kind of Preparation Method, and in particular to separable life using glass fibre as two-dimensional graphene/copper nano particles mixed structure of substrate
Biology sensor of thing molecule and preparation method thereof.
Background technology
It is most important for current biology sensor, high sensitivity, high stability, high efficiency.Highly sensitive original position
SERS technologies can in real time, quickly detect environment, pollution of agricultural products and its canceration of initiation, to pollution control and medical consultations
It is important Deng having the function that.At present, relevant progress is more slow, and main cause is highly sensitive bio-sensing equipment
Preparing for material is relatively difficult.
The separation of molecule under mixing polymolecular can be achieved in molecule separation, is conducive to more accurately detect molecule in mixing polymolecular
Species, has the function that important in environmental monitoring, medical diagnosis and life entity characterization etc..Adopted during separation to mixed solution
With paper chromatography, paper chromatography is the chromatography using paper as carrier.Stationary phase is generally the moisture adsorbed in paper fiber, mobile phase
For organic solvent not compatible with water；Also other materials of paper occlusion can be made as stationary phase, such as buffer solution, formamide etc..Will examination
Then sampling point is unfolded in closed groove with suitable solvent in one end of paper slip.After component moves a certain distance, each group
Divide displacement distance different, eventually form spot disconnected from each other.
What is utilized when being detected to molecule is the technology of Surface enhanced Raman scattering (SERS).Raman spectrum and red
External spectrum equally belongs to molecular vibration spectrum, can reflect the feature structure of molecule.But Raman scattering effect is very
Weak process, its general light intensity are only about the 10 of incident intensity-10.So Raman signal is all very weak, to adsorption species into
Row raman study is almost employed to certain enhancement effect.The viewpoint more universal at present on Surface enhanced Raman scattering be
The surface of SERS activity tends to produce enhanced local electric field, is that this is referred to as caused by surface plasma resonance vibration
Physics strengthens.And absorption of the molecule on metal often causes the change of molecular entergy level, or molecule to be inhaled with the transfer of electric charge
Being attached on special metallic surface structures point also causes to strengthen, and both of which is referred to as Chemical enhancement.In some special feelings
Under condition, people are also making great efforts the detection of progress individual molecule.
In recent years, with the fast development of laser technology, nanosecond science and technology and computer technology, SERS is at interface and table
The fields such as face science, material analysis, biology, medicine, food security, environmental monitoring and national security are widely applied.
SERS technologies not only have the advantages that the most of of Raman spectrum, using the teaching of the invention it is possible to provide the structural information of more rich chemical molecular, can be real
When real, in-situ investigation, and high sensitivity, data processing is simple, and accuracy rate is high, is very strong trace detection work
Tool.
Due to its without sample pretreatment, easy to operate, detection speed is fast, accuracy rate is high, instrument is portable the features such as, SERS
Detection plays positive effect in food security quickly detects, and illegally adds for example, SERS can be harmful to qualitative and quantitative analysis
Add in thing (such as melamine, tonyred), the additive (synthetic dyestuff in such as food) of excess Use overrun, fruits and vegetables
Pesticide residue and bacterium on foodstuff surface and virus etc..Obviously, SERS is expected to become a kind of quick point of common scene
Analysis method.However, the biology sensor that SERS is used at present is low there are sensitivity, preparation process is cumbersome, of high cost, it is difficult to detects
The shortcomings of mixed biologic molecule.
The content of the invention
The defects of to overcome the prior art, the present invention provides a kind of highly sensitive separable biology available in situ detection
The preparation method of sensor.
To achieve the above object, the technical scheme is that：
A kind of biology sensor of graphene/copper particle mixed structure, two dimension is attached with the upper surface of all-glass paper
The layer structure that graphene is mixed with copper nano particles.
Heretofore described all-glass paper is the tissue paper manufactured paper with pulp by the tiny glass fibre of diameter.
Heretofore described two-dimensional graphene is for one kind by carbon atom with sp2Hybridized orbit composition hexangle type is brilliant in honeycomb
The flat film of lattice, the two-dimensional material of only one carbon atom thickness.
Heretofore described nano particle is no more than 300 nanometers of minitype particle for size.
Preferably, the nano particle is that size is 50~150nm.
The preparation method of the biology sensor of a kind of graphene/copper particle mixed structure, using Vacuum Coating method in glass
Copper plating film in fibrous paper, makes the graphene of generation be deposited on the copper film using chemical vapour deposition technique, while makes copper film quilt
Copper nano particles layer is processed into, so that copper film forms the layer structure that two-dimensional graphene is mixed with copper nano particles.
Heretofore described Vacuum Coating method is under conditions of vacuum, and metal material is heated, when temperature exceedes gold
When belonging to the boiling point of material, heated metal material is drastically evaporated with gaseous state, is sprayed around with straight line；When running into barrier
Adhere to accumulation in body surface, form thin film.
Heretofore described chemical vapour deposition technique (abbreviation CVD method) is a kind of method of vapor-phase growing for preparing material,
It is one or more of compounds containing composition film element, elementary gas to be passed through the reative cell for being placed with base material, by sky
Between gas-phase chemical reaction depositing solid films on matrix surface technology.
When preferably, using Vacuum Coating method, vacuum condition is：Vacuum is 2 × 10-3~5 × 10-3Torr。
Heretofore described vacuum is the vacuum under ordinary meaning, and the as gas under vacuum state is thin
Degree." Torr " is pressure unit, 1Torr ≈ 133.322Pa=1.333mbar (millibar)=0.001315789473atm.
When preferably, using Vacuum Coating method, 135A is increased in evaporation current 3min.
Preferably, the thickness of the copper film is 100nm~300nm.
Preferably, the length and width dimensions of the copper film are 5cm × 5cm~20cm × 20cm.
Preferably, the step of chemical vapour deposition technique is that the all-glass paper for being coated with copper film is put into vacuum reaction
In stove, open vacuum pump and vacuumize and hydrogen is persistently injected in backward vacuum reaction stove, reheating continues after being warming up to preset temperature
Inject methane, constant temperature certain time after annealing.
Heretofore described annealing refers to dispelling substrate surface the process of the impurity such as oxide.
It is further preferred that stopping being passed through methane after annealing, cooled to room temperature can obtain graphene/copper particle and mix
Close the biology sensor of structure.
It is further preferred that stopping being passed through methane after annealing, continue to inject hydrogen, and hydrogen injection flow velocity is constant, then make
The biology sensor of graphene/copper particle mixed structure is taken out after vacuum reaction in-furnace temperature cooled to room temperature.
Still more preferably, after vacuum reaction in-furnace temperature is cooled to room temperature, stopping is passed through hydrogen and closes vacuum pump,
The external atmosphere pressure that air pressure is 0.9-1.0 times in air to vacuum reaction stove is injected into vacuum reaction stove again, then takes out stone
The biology sensor of black alkene/copper particle mixed structure.
Heretofore described external atmosphere pressure is the atmospheric pressure of vacuum reaction stove local environment.
It is further preferred that the vacuum after vacuum reaction stove evacuation is 3 × 10-3-3×10-6Torr.To remove stove
Active gases in chamber, keeps clean growing environment.
It is further preferred that the injection flow control of the hydrogen is 1-100sccm.
Unit " sccm " (Standard Cubic Centimeter per Minute) is to represent per minute in the present invention
Standard milliliters.
It is further preferred that the purity of the hydrogen is more than 99.99%.
It is further preferred that the preset temperature is 850~1050 DEG C.
It is further preferred that the injection flow control of the methane is 1-300sccm.
It is further preferred that the purity of the methane is more than 99.99%.
It is further preferred that the annealing time is 10~30min.
It is further preferred that the annealing temperature is 850~1050 DEG C.
Biology sensor prepared by a kind of above-mentioned preparation method.
A kind of application of above-mentioned biology sensor in mixed molecules are detected.
A kind of method of above-mentioned biology sensor detection mixed molecules, comprises the following steps：
(1) above-mentioned biology sensor is trimmed to list structure, is preset in one end of list structure, and apart from the end end
Baseline is drawn at distance；
(2) the solution point of mixed molecules is added at the baseline, dried；
(3) biology sensor after drying carries out presaturation processing；
(4) part below the baseline of the biology sensor after presaturation is handled, which is immersed in solvent, is unfolded；
(5) after each molecule is kept completely separate in mixed molecules, after taking-up biology sensor dries, the molecule after separation is carried out
Detection.
Heretofore described list structure, is preferably rectangular list structure, it is ensured that material is in list structure
It is upper to be uniformly unfolded.Baseline is drawn in one end of list structure, mixed molecules solution, baseline to the other end are coated on baseline
Between biology sensor material be in mixed molecules solution various materials carry out separated paths, since list structure has
Various materials, can be kept completely separate by certain length.
Heretofore described mixed molecules are the mixture of biomolecule, wherein, it is peculiar that biomolecule refers to organism
Each quasi-molecule, be organic matter.Such as crystal violet (CV), toluidine blue (TB) etc..
Heretofore described presaturation processing is the presaturation processing on ordinary meaning, the presaturation in paper chromatography
Processing includes first making saturation in solvent steam presaturation process container, then that the biology sensor after drying is put into steam is pre- full
With saturated process is carried out in process container.Its object is to：1. being the edge effect for reducing biology sensor, spot is set to correspond to more
Accurately；2. reducing the inferior separating effect that bad (such as edge is irregular) in prepared by biology sensor brings, separation effect is improved
Fruit.
Preferably, the presaturation time is 5-25min.
Heretofore described solvent is, when extraction separates, for the solvent of the different many kinds of substance of separating polar.
Preferably, the solvent is more than 99.0% ethanol solution for concentration.
It is further preferred that the solvent is the ethanol solution of concentration 99.5%.
The present invention key problem in technology be：
(1) thickness of electroless copper plating film is the key for preparing excellent biology sensor.The thickness of copper sheet will be blocked up to be given birth in CVD method
Copper nanostructured can not be formed during long graphene；The thickness of copper sheet it is excessively thin will in CVD method growth evaporating completely；On
State the Raman enhancing for being either way unfavorable for strengthening molecule.Therefore, when evaporating electroless copper plating film, can the thickness of copper plating film be to prepare
The key of excellent sensor.
(2) during CVD method grows graphene, the flow velocity of hydrogen and methane is controlled, the ratio of hydrogen and methane is
The key technology of good two-dimensional graphene can be grown.Rational hydrogen, whether the ratio of methane decides can grow
Go out the two-dimensional graphene at low defect peak.
(3) during CVD method grows graphene, can cycle annealing be to grow highly sensitive graphene/copper to receive
The key of the sensor of rice grain mixed structure.Determinant therein includes the time of cycle annealing and the temperature of cycle annealing
Degree, the longer growth for being conducive to graphene of the time of cycle annealing, but copper particle evaporating completely can be caused；The time of cycle annealing
It is shorter to cause that copper nanostructured cannot be formed, also it is unfavorable for the growth of graphene.Therefore, control cycle annealing temperature and when
Between be the key that can grow high sensitive sensor.
(4) when doing molecule separation it is noted that not allow determinand direct invasion into developping solution, otherwise the failure of an experiment,
Mixed molecules can not be isolated；On the other hand, during presaturation, can pre-saturated time control is good separation mixing
The key of testing molecule.
The beneficial effects of the invention are as follows：
1. the growth temperature of graphene accurately controls；
2. the graphene defect peak of growth is low, there is high crystal quality；
3. the graphene size of growth is only limited the large area deposition, it can be achieved that graphene by CVD cavitys；
4. using evaporating, splash growth copper particle cost is low, and can effectively control the copper film size of generation.
5. there is graphene/copper particle mixed structure after the metallic particles of growth high chemisorbed and physics to strengthen
Mechanism, is conducive to the detection of molecule；
6. the present invention can generate two-dimensional graphene/copper nano particles structure at the same time using CVD method, reduce technique stream
Journey, reduces production cost.
7. the separation and detection of biomolecule can be achieved at the same time in the hair sensor that the biology after the completion of preparing passes.
8. method is simply controllable, of low cost, application value is high.
Brief description of the drawings
Fig. 1 be two-dimensional graphene/copper nano particles biology sensor in two-dimensional graphene and copper nano particles mixing
The SEM figures of structure；
Fig. 2 is Raman detection figure of the two-dimensional graphene/copper nano particles glass fiber material to CV molecules；
Fig. 3 is Raman detection figure of the two-dimensional graphene/copper nano particles glass fiber material to TB molecules；
Fig. 4 is the technique preparation flow figure of two-dimensional graphene/copper nanometer biology sensor.
Embodiment
Below in conjunction with the accompanying drawings and specific embodiment the invention will be further described.
Embodiment 1
The preparation method of the biology sensor of graphene/copper nano particles, as shown in Figure 4.
1. cutting the blank glass fiber paper of 5cm × 15cm with scissors, the copper foil of certain mass is cut.
2. opening evaporation splash instrument, the copper of certain mass is put into evaporation boat, glass fibre is then put into evaporation
In instrument, evaporation splash instrument is shut, checks whether air-tightness is good.
3. opening instrument operating switch, mechanical pump is opened successively, bypass valve, molecular pump, evaporator is evacuated to 3 ×
10-3Torr。
4. after vacuumizing, evaporation button is opened, slowly increase evaporation current to 135A, persistently evaporation one minute, so
Evaporation button is closed afterwards.Aspiration pump is closed after waiting ten minutes, evaporator is opened and takes out glass fiber material.
5. the all-glass paper after drying is put into tube furnace, and tube furnace is shut, check air-tightness.
6. open vacuum pump is evacuated to end vacuum state 3 × 10 by the air pressure of tube furnace-6Hold in the palm (Torr)；
7. keep vacuum state 3 × 10-6Torr (the vacuum effect of 15 minutes is to dispel quartz only) after 15 minutes, by stone
The air pressure of English pipe 3 is raised to 3 × 10-3Torr；
8. hydrogen flowmeter is set as 20sccm, by hydrogen injection vacuum chamber；
After 9. tubular type furnace temperature is warming up to 950 DEG C, start to be passed through methane gas, flow meter settings 80sccm, constant temperature
20min anneals；
10. close methane gas flowmeter and tubular type furnace temperature is quickly down to room temperature with the speed of 50 DEG C/min；
11. close hydrogen flowmeter and vacuum pump；
12. opening valve, quartz ampoule air pressure is filled to an atmospheric pressure state with air；
13. opening quartz ampoule vacuum interface, the biology sensor for having formed graphene/copper nano particles is taken out.
The middle two-dimensional graphene of the biology sensor of graphene/copper nano particles of preparation and the mixing knot of copper nano particles
Scanning electron microscope (SEM) figure of structure is as shown in Figure 1.
Using the method for the biology sensor detection mixed molecules of above-mentioned graphene/copper nano particles, comprise the following steps：
(1) biology sensor of above-mentioned 5cm × 15cm is removed, in one end of biology sensor material, and apart from the end end
Baseline is drawn at 1cm；
(2) solution of the solution of CV, TB mixed molecules, the solution of CV biomolecule and TB biomolecule is coated in base respectively
At the diverse location of line, dry；
(3) biology sensor dried is put into the beaker of the ethanol containing solvent (99.5% ethanol solution)
Carry out 15min presaturations；
(4) part below biology sensor material baseline is immersed in 99.5% ethanol solution and is unfolded；
(5) after CV, TB are kept completely separate, biology sensor material is taken out, after drying, biomolecule letter is carried out using Raman
Number detection.
As shown in Figure 2,3, Fig. 2 is to various concentrations 10 to testing result-6-10-4The testing result of M CV molecules, Fig. 3 are pair
Various concentrations 10-6-10-5The testing result of M TB molecules.It can be seen that using above-mentioned graphene/copper nano particles from Fig. 2,3
Biology sensor high sensitivity, test limit is low.
Although above-mentioned be described the embodiment of the present invention with reference to attached drawing, not to invention protection domain
Limitation, those skilled in the art should understand that, on the basis of technical scheme, those skilled in the art are not required to
Make the creative labor the various modifications that can be made or deformation is still within the scope of the present invention.
Claims (10)
1. a kind of graphene/copper particle mixed structure separates the biology sensor of biomolecule, it is characterized in that, in glass fibre
The upper surface of paper is attached with the layer structure that two-dimensional graphene is mixed with copper nano particles.
2. biology sensor as claimed in claim 1, it is characterized in that, a diameter of 50 ~ 150nm of the copper nano particles.
3. biology sensor as claimed in claim 1, it is characterized in that, preparation method is, using Vacuum Coating method in glass fibers
Copper plating film on paper is tieed up, the graphene of generation is deposited on the copper film using chemical vapour deposition technique, while located copper film
Copper nano particles layer is managed into, so that copper film forms the layer structure that two-dimensional graphene is mixed with copper nano particles.
4. biology sensor as claimed in claim 3, it is characterized in that, during using Vacuum Coating method, vacuum condition is：Vacuum
For 2 × 10-3~5×10-3Torr；
Or, during using Vacuum Coating method, 135A is increased in 3 min of evaporation current；
Or, the thickness of the copper film is 100nm ~ 300nm.
5. biology sensor as claimed in claim 3, it is characterized in that, the step of chemical vapour deposition technique is to be coated with
The all-glass paper of copper film is put into vacuum reaction stove, is opened vacuum pump and is vacuumized in backward vacuum reaction stove and persistently injects hydrogen
Gas, reheating persistently inject methane, constant temperature certain time after annealing after being warming up to preset temperature.
6. biology sensor as claimed in claim 5, it is characterized in that, stop being passed through methane, cooled to room temperature after annealing
The biology sensor of graphene/copper particle mixed structure can be obtained；
Or, stop being passed through methane after annealing, continue to inject hydrogen, and hydrogen injection flow velocity is constant, then make warm in vacuum reaction stove
The biology sensor of graphene/copper particle mixed structure is taken out after degree cooled to room temperature；
Or, the vacuum after vacuum reaction stove evacuation is 3 × 10-3-3×10-6Torr；To remove the active gases in furnace chamber,
Keep clean growing environment；
Or, the injection flow control of the hydrogen is 1-100sccm；
Or, the purity of the hydrogen is more than 99.99%；
Or, the preset temperature is 850 ~ 1050 DEG C；
Or, the injection flow control of the methane is 1-300sccm；
Or, the purity of the methane is more than 99.99%；
Or, the annealing time is 10 ~ 30min；
Or, the annealing temperature is 850 ~ 1050 DEG C.
A kind of 7. application of the biology sensor in mixed molecules are detected as described in any in claim 1 ~ 6.
8. a kind of method of biology sensor detection mixed molecules as described in any in claim 1 ~ 6, it is characterized in that, including
Following steps：
（1）Biology sensor as described in any in claim 1 ~ 6 is trimmed to list structure, in one end of list structure,
And draw baseline at the end end pre-determined distance；
（2）The solution point of mixed molecules is added at the baseline, is dried；
（3）Biology sensor after drying carries out presaturation processing；
（4）Part below the baseline of biology sensor after presaturation is handled, which is immersed in solvent, is unfolded；
（5）After each molecule is kept completely separate in mixed molecules, after taking-up biology sensor dries, the molecule after separation is examined
Survey.
9. method as claimed in claim 8, it is characterized in that, the presaturation time is 5-25min；
Or, the solvent is more than 99.0% ethanol solution for concentration.
10. method as claimed in claim 9, it is characterized in that, the solvent is the ethanol solution of concentration 99.5%.
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| US9278855B2 (en) * | 2011-05-27 | 2016-03-08 | Drexel University | Flexible SERS substrates with filtering capabilities |
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| CN104777151A (en) * | 2015-04-23 | 2015-07-15 | 西北工业大学 | Ultra-sensitive SERS substrate and preparation method thereof |
| CN105651756A (en) * | 2016-01-04 | 2016-06-08 | 山东师范大学 | Raman enhanced base for amplifying raman signal, and preparation method and application thereof |
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