CN106442464A - Preparing method of silicon wafer/reduced graphene/gold nanocomposite material - Google Patents
Preparing method of silicon wafer/reduced graphene/gold nanocomposite material Download PDFInfo
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- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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Abstract
The invention relates to the field of graphene/precious metal composite materials, and provides a preparing method of a silicon wafer/reduced graphene/gold nanocomposite material. By means of the preparing method, gold nano structures which are different in morphology and distributed uniformly can be obtained on the surface of graphene. The composite material serves as a surface-enhanced Raman active base, is used for detecting small organic molecule 4-aminothiophenol (4-ATP) and expresses high Raman activity, the detection concentration of 4-ATP can reach 10<-7>M, and trace detection of the small organic molecule can be achieved.
Description
Technical field
The present invention relates to Graphene/noble metal composite-material field, more specifically, is related to a kind of poly- using pyrroles's gas phase
Conjunction method in graphene oxide/polymer brush composite material surface regulation and control gold nano structure and ultimately forms reduced graphene/gold
The preparation method of composite.
Background technology
Graphene/noble metal (gold, silver, palladium etc.) nano composite material be considered as most have application prospect composite it
One, Graphene/noble metal nano composite combines many excellent properties of noble metal nanometer material and grapheme material, such as
The photoelectric characteristic of noble metal nanometer material, the bigger serface of grapheme material, high mechanical properties, satisfactory electrical conductivity and biology are simultaneous
Capacitive etc..While the excellent specific property of Graphene can also produce synergistic enhancing effect to the precious metal material for loading, so as to significantly carry
The overall performance of high composite.This causes Graphene/noble metal composite nano materials in surface enhanced raman spectroscopy
There is fabulous application prospect in terms of (Surface-enhanced Raman scattering, SERS).Up to the present, lead to
Often preparing Graphene/noble metal nano composite mainly has following several method:(1) wet chemistry method:The method be by graphite
After alkene and noble metal precursor body Ar ion mixing, in the presence of reducing agent, by noble metal precursor body ion in graphenic surface also
Original becomes corresponding noble metal nano particles.(2) solvent-thermal method:The method be exactly with other liquid such as water or polyhydric alcohol as solvent,
By noble metal precursor body (AgNO3, HAuCl4, PdCl2Deng) and graphene oxide solution mixing, in a kettle., temperature is 100-
Under conditions of 1000 DEG C, by means of the material (as reducing agent or solvent itself) in solution system by noble metal precursor body ion also
Original becomes noble metal nano particles, so as to form Graphene/noble metal nano complex.(3) electrochemical process:The method first has to
Electrode surface deposited graphite alkene, then by electrochemical method in graphenic surface depositing noble metal nanoparticle.(4) self assembly
Method:The method needs to carry out chemical treatment to graphenic surface first, can adsorb noble metal nano in graphenic surface connection
Then pre-synthesis noble metal nano particles are adsorbed onto graphenic surface by the functional group of particle.
Content of the invention
But for the method for Graphene/noble metal nano composite is prepared at present, by traditional method very
The pattern of difficult control graphenic surface noble metal nano particles;While it is also difficult to avoid that some chemical substances hinder electron transfer,
And then reduce the surface enhanced raman spectroscopy performance of Graphene/noble metal composite-material.
In view of be difficult at present regulate and control the pattern of noble metal nano structure in graphenic surface, the invention provides a kind of new
The new method of different-shape and the gold nano structure that is evenly distributed is obtained on reduced graphene surface.The present inventor etc. is through deeply
Research, finally found that:By " self-initiating photografting polymerization technology " in graphene oxide (graphite oxide, GO) surface shape
Become poly 4 vinyl pyridine (poly (4-vinylpyridene, P4VP)) to brush, adsorb gold chloride (HAuCl4) after, then will absorption
Have in the graphene oxide/poly 4 vinyl pyridine immersion chromium solution of gold chloride, adsorb the AuCl on P4VP brush strand4 -
Ion itself can be reduced into golden (Au) nano junction while oxidizable pyrrole is become polypyrrole (polypyrrole, PPy)
Structure, so as to form GO/P4VP/PPy-Au composite.We are by controlling the response time, it is possible to obtain the Jenner of different-shape
Rice structure.Last GO/P4VP/PPy-Au composite processes (500 DEG C) by high temperature anaerobic, remove P4VP polymer brush with
PPy organic polymer, GO is converted into reduced graphene (reduced graphite oxide, rGO), so as to obtain reducing graphite
Alkene/gold (rGO/Au) composite.
Idea of the invention be as follows,
A kind of preparation method of silicon chip/reduced graphene/Jenner's nano composite material, including step 1, step 2, step 3 and step
4,
Step 1:There is the silicon chip of silica dioxide coating as substrate with surface, substrate aminofunctional obtains amido modified silicon
Piece, the ethanol solution of graphene oxide (GO) is dropped on silica gel seal, is transferred to GO using seal stamp transfer method described
Amido modified silicon chip on, obtain GO modification silicon chip (silicon chip/GO);
Step 2:Silicon chip/the GO of gained is dipped in the seal pipe containing 4-vinylpridine (P4VP) monomer, uses ultraviolet light
30-180min is irradiated, reaction is taken out silicon chip and rinsed with chloroformic solution after terminating, obtain silicon chip/graphene oxide/poly- 4- ethylene
Yl pyridines brush (silicon chip/GO/P4VP brush);
Step 3:The silicon chip of gained/GO/P4VP brush is immersed in aqueous solution of chloraurate, soak time is 6-18h, after taking-up,
It is washed with deionized, obtains being adsorbed with AuCl4 -The silicon chip of ion/GO/P4VP brush, then the silicon chip of gained/GO/P4VP brush is put
Put in the hermetic container containing pyrroles, and the silicon chip/GO/P4VP brush is not contacted with pyrroles, reacts 1-8h, you can obtain silicon
Piece/graphene oxide/poly 4 vinyl pyridine brush/polypyrrole-metal/composite material (silicon chip/GO/P4VP/PPy-Au composite wood
Material);
Step 4:By the silicon chip of gained/GO/P4VP/PPy-Au composite at 400-800 DEG C, anaerobic processes 0.5-3h, obtains
Silicon chip/reduced graphene/metal/composite material (silicon chip/rGO/Au composite).
The invention has the beneficial effects as follows:The silicon chip of gained/rGO/Au composite is used as surface reinforced Raman active substrate
For organic molecule 4- aminothiophenol (4-ATP) is detected, extremely strong Raman active is shown, to 4-ATP small molecule
Detectable concentration can reach 10-7M, it is possible to achieve the trace detection to organic molecule.
Description of the drawings
Fig. 1 is the synthetic route chart of silicon chip/GO/P4VP/PPy-Au composite;
Fig. 2 is schemed for the XPS of silicon chip/GO;
Fig. 3 is the XPS figure of silicon chip/GO/P4VP brush;
Fig. 4 is schemed for the SEM of silicon chip/GO/P4VP/PPy-Au composite;
Fig. 5 is schemed for the XPS of silicon chip/GO/P4VP/PPy-Au composite;
Fig. 6 is schemed for the SEM of silicon chip/rGO/Au composite;
Fig. 7 is the Raman spectrogram of the 4-ATP molecule in silicon chip/rGO/Au composite material surface of variable concentrations.
Specific embodiment
Below, the present invention is described in detail.
The present invention is a kind of preparation method of silicon chip/reduced graphene/Jenner's nano composite material, including step 1, step 2,
Step 3 and step 4,
Step 1:There is the silicon chip of silica dioxide coating as substrate with surface, substrate aminofunctional obtains amido modified silicon
Piece, the ethanol solution of graphene oxide (GO) is dropped on silica gel seal, is transferred to GO using seal stamp transfer method described
Amido modified silicon chip on, obtain GO modification silicon chip (silicon chip/GO);
Step 2:Silicon chip/the GO of gained is dipped in the seal pipe containing 4-vinylpridine (P4VP) monomer, uses ultraviolet light
30-180min is irradiated, reaction is taken out silicon chip and rinsed with chloroformic solution after terminating, obtain silicon chip/graphene oxide/poly- 4- ethylene
Yl pyridines brush (silicon chip/GO/P4VP brush);
Step 3:The silicon chip of gained/GO/P4VP brush is immersed in aqueous solution of chloraurate, soak time is 6-18h, after taking-up,
It is washed with deionized, obtains being adsorbed with AuCl4 -The silicon chip of ion/GO/P4VP brush, then the silicon chip of gained/GO/P4VP brush is put
Put in the hermetic container containing pyrroles, and the silicon chip/GO/P4VP brush is not contacted with pyrroles, reacts 1-8h, you can obtain silicon
Piece/graphene oxide/poly 4 vinyl pyridine brush/polypyrrole-metal/composite material (silicon chip/GO/P4VP/PPy-Au composite wood
Material);
Step 4:By the silicon chip of gained/GO/P4VP/PPy-Au composite at 400-800 DEG C, anaerobic processes 0.5-3h, obtains
Silicon chip/reduced graphene/metal/composite material (silicon chip/rGO/Au composite).
In the present invention, the synthetic route chart of silicon chip/GO/P4VP/PPy-Au composite is as shown in Figure 1.
In above-mentioned steps 1, substrate aminofunctional is obtained amido modified silicon chip, the method for functionalization has no special limit
Fixed, generally can be obtained by substrate is dipped in the silane coupler solution containing amino.Silane coupler containing amino is simultaneously
It is not particularly limited, 3- aminopropyl triethoxysilane, 3- aminopropyl-trimethoxy silane, γ-aminopropyltriethoxy two can be selected
Any one in Ethoxysilane and γ-aminopropyltriethoxy dimethoxysilane.Solvent in silane coupler solution, has no
It is particularly limited to, can such as selects benzene.Silane coupled agent concentration, is not particularly limited, and can be 3-30wt%.
In above-mentioned steps 1, in the ethanol solution of graphene oxide (GO), the concentration of GO is not particularly limited, usually
0.01-0.05mg/mL, within this range, GO can be uniformly dispersed in ethanol solution concentration.Using seal stamp transfer method by GO
Being transferred on the silicon chip with amino, as substantial amounts of oxy radical is carried on GO, can interact with the amino on silicon chip, from
And GO is firmly adhered on silicon chip.
In above-mentioned steps 3, the concentration of aqueous solution of chloraurate is not particularly limited, generally in 0.05wt%-2wt%;Absorption
There is AuCl4 -The poly 2 vinyl pyridine brush (P2VP brush) of ion is placed in the hermetic container containing chromium solution, and the P2VP
Brush is not contacted with pyrroles, and this point is extremely important.As the P2VP brush is not contacted with pyrroles, AuCl is adsorbed with4 -The P2VP of ion
AuCl in brush4 -Pyrroles's vapor-phase oxidation is polymerized and obtains polypyrrole by ion, and AuCl4 -Ion itself is reduced into not similar shape
The Au nanostructured of looks.
Above-mentioned steps 1-4, if reaction temperature is not particularly illustrated, for 25-35 DEG C of room temperature condition.In above-mentioned steps 2,
The wavelength of the ultraviolet light for being used is 350nm.
Below, by the following examples present invention more particularly described below.Here, embodiment is merely to illustrate the present invention, no
It is construed that limiting the scope of the invention.It is can to carry out in the case of without departing from its spirit and scope to implement the present invention
Various changes and modifications.These changes and improvement are within the scope of the appended claims, it should be understood that it is the one of the present invention to become
Part.
(embodiment 1)
Step 1:First, surface is had the silicon chip 3- aminopropyl triethoxysilane of the immersion containing 5% of silica dioxide coating
In toluene solution, ultrasonic reaction 2 hours, so as to obtain amido modified silicon chip.By 0.025mg/mL graphene oxide (GO)
Ethanol solution is dropped on silica gel seal, using seal stamp transfer method, GO is transferred on the silicon chip with amino, is spontaneously dried, i.e.,
(silicon chip/GO) of GO modification is obtained.
Fig. 2 is the XPS spectrum of silicon chip/GO, four four peaks of characteristic peak of in figure 289.1,287.7,286.6,284.6eV, they
Carboxyl (COO), the carbonyl (C=O) of GO is corresponded respectively to, the C-C/C=C group in epoxide group and aromatic rings, so as to prove
GO has successfully been grafted to silicon chip surface.
Step 2:Silicon chip/the GO of gained is dipped in the seal pipe containing 4-vinylpridine monomer, under room temperature, uses ultraviolet light
(wavelength 350nm) irradiates 2 hours, after reaction terminates, is rinsed with chloroform repeatedly and is polymerized with removing the non-grafted P4VP to GO surface
Thing, obtains silicon chip/graphene oxide/poly 4 vinyl pyridine brush (silicon chip/GO/P4VP brush).
Fig. 3 is the XPS figure of silicon chip/GO/P4VP brush, and in figure occurs in that obvious N 1s peak, and which belongs to P4VP, so as to prove
P4VP brush has successfully been grafted to GO surface.
Step 3:Silicon chip/GO/P4VP is brushed in gold chloride (HAuCl4) soak 12 hours in aqueous solution (1%wt), then take out
It is washed with deionized, removes unadsorbed HAuCl4.HAuCl will be subsequently adsorbed with4Silicon chip/GO/P4VP brush be placed into containing
The hermetic container of pyrroles, and the silicon chip/GO/P4VP brush contact with pyrroles, and reaction 3 hours obtains silicon chip/graphite oxide
Alkene/poly 4 vinyl pyridine brush/polypyrrole-metal/composite material (silicon chip/GO/P4VP/PPy-Au composite).
Fig. 4 (A) is schemed for the SEM of silicon chip/GO/P4VP/PPy-Au composite, it is known that obtain flowers shape Au structure.
Fig. 5 is schemed for the XPS of silicon chip/GO/P4VP/PPy-Au composite, and in figure shows obvious Au4f peak, so as to prove
HAuCl4It has been reduced into Au.
Step 4:Silicon chip/GO/P4VP/PPy-Au composite is processed 2 hours in 500 DEG C of high temperature anaerobics, in this process
P4VP brush and PPy Organic substance will be removed, and GO is then changed into rGO, so as to obtain silicon chip/rGO/Au composite.
Fig. 6 (A) is silicon chip/rGO/Au composite SEM figure, although it can be seen that eliminating P4VP and PPy is organic
Thing, the pattern of silicon chip/rGO/Au is held essentially constant.
(embodiment 2)
Step 1 and step 2 are identical with embodiment.
Step 3:Silicon chip/GO/P4VP is brushed in gold chloride (HAuCl4) soak 12 hours in aqueous solution (1%wt), then take out
It is washed with deionized, removes unadsorbed HAuCl4.HAuCl will be subsequently adsorbed with4P4VP brush be placed into containing chromium solution
Hermetic container, and the silicon chip/GO/P4VP brush contact with chromium solution, reaction 7 hours, that is, obtain silicon chip/graphite oxide
Alkene/poly 4 vinyl pyridine brush/polypyrrole-metal/composite material (silicon chip/GO/P4VP/PPy-Au composite).
Fig. 4 (B) is schemed for the SEM of silicon chip/GO/P4VP/PPy-Au composite, it is known that obtain coralliform gold nano structure.
Step 4:Silicon chip/GO/P4VP/PPy-Au composite is processed 2 hours in 500 DEG C of high temperature anaerobics, in this process
P4VP brush and PPy Organic substance will be removed, and GO is then changed into rGO, so as to obtain silicon chip/rGO/Au composite.
Fig. 6 (B) is silicon chip/rGO/Au composite SEM figure, although it can be seen that eliminating P4VP and PPy is organic
Thing, the pattern of silicon chip/rGO/Au is held essentially constant.
(reference example)
Silicon chip/rGO/Au composite is used as Raman substrate detection 4- aminothiophenol (4-ATP)
In Raman test process, we select the silicon chip/rGO/Au composite of 1 gained of embodiment as Raman substrate material
Material, prepares the 4-ATP ethanol solution of variable concentrations first, then rGO/Au composite is dipped in 4-ATP solution, and 6 is little
When after take out, be washed with deionized 3 times, finally dried up with highly purified nitrogen stream, for Raman test.Shown in Fig. 7 not
With concentration 4-ATP silicon chip/rGO/Au composite material surface Raman spectrum ((a) 10-4M, (b) 10-5M, (c) 10-6M, (d)
10-7M), even if it can be seen that 4-ATP molecular concentration as little as 10-7M, Raman spectrum still can show stronger characteristic peak,
So as to prove that silicon chip/rGO/Au composite is a kind of excellent Raman active substrate material, organic molecule can be realized
Trace detection.
Claims (2)
1. a kind of preparation method of silicon chip/reduced graphene/Jenner's nano composite material, including step 1, step 2, step 3 and step
Rapid 4,
Step 1:There is the silicon chip of silica dioxide coating as substrate with surface, substrate aminofunctional obtains amido modified silicon
Piece, the ethanol solution of graphene oxide (GO) is dropped on silica gel seal, is transferred to GO using seal stamp transfer method described
Amido modified silicon chip on, obtain GO modification silicon chip (silicon chip/GO);
Step 2:Silicon chip/the GO of gained is dipped in the seal pipe containing 4-vinylpridine (P4VP) monomer, uses ultraviolet light
30-180min is irradiated, reaction is taken out silicon chip and rinsed with chloroformic solution after terminating, obtain silicon chip/graphene oxide/poly- 4- ethylene
Yl pyridines brush (silicon chip/GO/P4VP brush);
Step 3:The silicon chip of gained/GO/P4VP brush is immersed in aqueous solution of chloraurate, soak time is 6-18h, after taking-up,
It is washed with deionized, obtains being adsorbed with AuCl4 -The silicon chip of ion/GO/P4VP brush, then the silicon chip of gained/GO/P4VP brush is put
Put in the hermetic container containing pyrroles, and the silicon chip/GO/P4VP brush is not contacted with pyrroles, reacts 1-8h, you can obtain silicon
Piece/graphene oxide/poly 4 vinyl pyridine brush/polypyrrole-metal/composite material (silicon chip/GO/P4VP/PPy-Au composite wood
Material);
Step 4:By the silicon chip of gained/GO/P4VP/PPy-Au composite at 400-800 DEG C, anaerobic processes 0.5-3h, obtains
Silicon chip/reduced graphene/metal/composite material (silicon chip/rGO/Au composite).
2. the preparation method of silicon chip/reduced graphene/Jenner's nano composite material according to claim 1, described substrate
Aminofunctional, is obtained by substrate is dipped in the silane coupler solution containing amino.
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TWI707974B (en) * | 2019-10-03 | 2020-10-21 | 國立高雄大學 | Molecular sensing substrate having metal ions bonded-graphene oxide or reduced graphene oxide and manufacturing method thereof |
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