CN106442464B - A kind of preparation method of silicon wafer/reduced graphene/Jenner's nano composite material - Google Patents
A kind of preparation method of silicon wafer/reduced graphene/Jenner's nano composite material Download PDFInfo
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- CN106442464B CN106442464B CN201610859268.XA CN201610859268A CN106442464B CN 106442464 B CN106442464 B CN 106442464B CN 201610859268 A CN201610859268 A CN 201610859268A CN 106442464 B CN106442464 B CN 106442464B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- 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
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
Abstract
The present invention relates to the present invention relates to graphene/noble metal composite-material fields, a kind of preparation method of silicon wafer/reduced graphene/Jenner's nano composite material is provided.Preparation method provided by the invention can obtain different-shape and the gold nano structure that is evenly distributed on the surface of graphene.Resulting composite material, for detecting small organic molecule 4- aminothiophenol (4-ATP), shows extremely strong Raman active, can achieve 10 to the detectable concentration of 4-ATP small molecule as surface reinforced Raman active substrate‑7The trace detection to small organic molecule may be implemented in M.
Description
Technical field
The present invention relates to graphene/noble metal composite-material fields, more specifically, are related to a kind of poly- using pyrroles's gas phase
Conjunction method is in graphene oxide/polymer brush composite material surface regulation gold nano structure and ultimately forms reduced graphene/gold
The preparation method of composite material.
Background technique
Graphene/noble metal (gold, silver, palladium etc.) nanocomposite be considered as most have application prospect composite material it
One, graphene/noble metal nano composite material 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 strength, satisfactory electrical conductivity and biology are simultaneous
Capacitive etc..The excellent characteristics of graphene can also generate synergistic enhancing effect to the precious metal material of load simultaneously, to significantly mention
The overall performance of high composite material.This makes graphene/noble metal composite nano materials in Surface enhanced Raman scattering
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 material is mainly the following method: (1) wet chemistry method: this method is by graphite
After alkene and noble metal precursor body Ar ion mixing, under the action of reducing agent, on the surface of graphene also by noble metal precursor body ion
Original is at corresponding noble metal nano particles.(2) solvent-thermal method: this method be exactly using other liquid such as water or polyalcohol as solvent,
By noble metal precursor body (AgNO3, HAuCl4, PdCl2Deng) and graphene oxide solution mixing, in a kettle, temperature 100-
Under conditions of 1000 DEG C, by means of the substance (such as reducing agent or solvent itself) in solution system by noble metal precursor body ion also
Original is at noble metal nano particles, to form graphene/noble metal nano compound.(3) electrochemical process: this method first has to
Electrode surface deposits graphene, then passes through electrochemical method depositing noble metal nanoparticle on the surface of graphene.(4) self assembly
Method: this method needs first to be chemically treated graphene surface, and connection can adsorb noble metal nano on the surface of graphene
Then pre-synthesis noble metal nano particles are adsorbed onto graphene surface by the functional group of particle.
Summary of the invention
However for preparing graphene/noble metal nano composite material method at present, very by traditional method
The pattern of graphene surface noble metal nano particles difficult to control；It is also difficult to avoid that certain chemical substances hinder electronics transfer simultaneously,
And then reduce graphene/noble metal composite-material Surface enhanced Raman scattering performance.
In view of being difficult to regulate and control the pattern of noble metal nano structure on the surface of graphene at present, the present 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 inventors of the present invention are by deeply
Research, finally found that: by " self-initiating photografting polymerization technology " in graphene oxide (graphite oxide, GO) surface shape
It is brushed at poly 4 vinyl pyridine (poly (4-vinylpyridene, P4VP)), adsorbs gold chloride (HAuCl4) after, then will absorption
There is graphene oxide/poly 4 vinyl pyridine of gold chloride to immerse in chromium solution, the AuCl being adsorbed on P4VP brush strand4 -
Ion itself can be reduced into golden (Au) nano junction while by oxidizable pyrrole at polypyrrole (polypyrrole, PPy)
Structure, to form GO/P4VP/PPy-Au composite material.We can obtain the Jenner of different-shape by the control reaction time
Rice structure.Last GO/P4VP/PPy-Au composite material by high temperature anaerobic processing (500 DEG C), remove P4VP polymer brush with
PPy organic polymer, GO are converted into reduced graphene (reduced graphite oxide, rGO), to obtain reduction graphite
Alkene/gold (rGO/Au) composite material.
The gist of the invention be it is as follows,
A kind of preparation method of silicon wafer/reduced graphene/Jenner's nano composite material, including step 1, step 2, step 3 and
Step 4,
Step 1: having the silicon wafer of silica dioxide coating as substrate using surface, substrate aminofunctional obtains amido modified
Silicon wafer, the ethanol solution of graphene oxide (GO) is dripped on silica gel seal, is transferred to GO using seal stamp transfer method
On the amido modified silicon wafer, the silicon wafer (silicon wafer/GO) of GO modification is obtained；
Step 2: resulting silicon wafer/GO being dipped into the seal pipe containing 4-vinylpridine (P4VP) monomer, with purple
Outer light irradiates 30-180min, takes out silicon wafer after reaction and is rinsed with chloroformic solution, obtains silicon wafer/graphene oxide/poly- 4-
Vinylpyridine brush (silicon wafer/GO/P4VP brush)；
Step 3: resulting silicon wafer/GO/P4VP brush being immersed in aqueous solution of chloraurate, soaking time 6-18h takes out
Afterwards, it is washed with deionized, obtains being adsorbed with AuCl4 -The silicon wafer of ion/GO/P4VP brush, then by resulting silicon wafer/GO/P4VP
Brush is placed in the closed container containing pyrroles, and the silicon wafer/GO/P4VP brush is not contacted with pyrroles, is reacted 1-8h, be can be obtained
Silicon wafer/graphene oxide/poly 4 vinyl pyridine brush/polypyrrole-metal/composite material (silicon wafer/GO/P4VP/PPy-Au composite wood
Material)；
Step 4: by resulting silicon wafer/GO/P4VP/PPy-Au composite material at 400-800 DEG C, anaerobic handles 0.5-3h,
Obtain silicon wafer/reduced graphene/metal/composite material (silicon wafer/rGO/Au composite material).
The beneficial effects of the present invention are: resulting silicon wafer/rGO/Au composite material is as surface reinforced Raman active substrate
For detecting small organic molecule 4- aminothiophenol (4-ATP), extremely strong Raman active is shown, to 4-ATP small molecule
Detectable concentration can achieve 10-7The trace detection to small organic molecule may be implemented in M.
Detailed description of the invention
Fig. 1 is silicon wafer/GO/P4VP/PPy-Au composite material synthetic route chart；
Fig. 2 is silicon wafer/GO XPS figure；
Fig. 3 is silicon wafer/GO/P4VP brush XPS figure；
Fig. 4 is silicon wafer/GO/P4VP/PPy-Au composite material SEM figure；
Fig. 5 is silicon wafer/GO/P4VP/PPy-Au composite material XPS figure；
Fig. 6 is silicon wafer/rGO/Au composite material SEM figure；
Fig. 7 is the 4-ATP molecule of various concentration in silicon wafer/rGO/Au composite material surface raman spectrum.
Specific embodiment
In the following, the present invention is described in detail.
The present invention be a kind of silicon wafer/reduced graphene/Jenner's nano composite material preparation method, including step 1, step 2,
Step 3 and step 4,
Step 1: having the silicon wafer of silica dioxide coating as substrate using surface, substrate aminofunctional obtains amido modified
Silicon wafer, the ethanol solution of graphene oxide (GO) is dripped on silica gel seal, is transferred to GO using seal stamp transfer method
On the amido modified silicon wafer, the silicon wafer (silicon wafer/GO) of GO modification is obtained；
Step 2: resulting silicon wafer/GO being dipped into the seal pipe containing 4-vinylpridine (P4VP) monomer, with purple
Outer light irradiates 30-180min, takes out silicon wafer after reaction and is rinsed with chloroformic solution, obtains silicon wafer/graphene oxide/poly- 4-
Vinylpyridine brush (silicon wafer/GO/P4VP brush)；
Step 3: resulting silicon wafer/GO/P4VP brush being immersed in aqueous solution of chloraurate, soaking time 6-18h takes out
Afterwards, it is washed with deionized, obtains being adsorbed with AuCl4 -The silicon wafer of ion/GO/P4VP brush, then by resulting silicon wafer/GO/P4VP
Brush is placed in the closed container containing pyrroles, and the silicon wafer/GO/P4VP brush is not contacted with pyrroles, is reacted 1-8h, be can be obtained
Silicon wafer/graphene oxide/poly 4 vinyl pyridine brush/polypyrrole-metal/composite material (silicon wafer/GO/P4VP/PPy-Au composite wood
Material)；
Step 4: by resulting silicon wafer/GO/P4VP/PPy-Au composite material at 400-800 DEG C, anaerobic handles 0.5-3h,
Obtain silicon wafer/reduced graphene/metal/composite material (silicon wafer/rGO/Au composite material).
Silicon wafer/GO/P4VP/PPy-Au composite material synthetic route chart is as shown in Figure 1 in the present invention.
In above-mentioned steps 1, substrate aminofunctional is obtained into amido modified silicon wafer, functionalized method has no special limit
It is fixed, it can usually be obtained by the way that substrate to be dipped into amino-containing silane coupler solution.Amino-containing silane coupling agent is simultaneously
It is not particularly limited, can choose 3- aminopropyl triethoxysilane, 3- aminopropyl-trimethoxy silane, γ-aminopropyltriethoxy two
Any one in Ethoxysilane and γ-aminopropyltriethoxy dimethoxysilane.Solvent in silane coupler solution, has no
It is particularly limited to, for example benzene can be selected.Silane coupling agent concentration, is not particularly limited, and can be 3-30wt%.
In above-mentioned steps 1, the concentration of GO is not particularly limited in the ethanol solution of graphene oxide (GO), 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
It is transferred on the silicon wafer with amino, due to that, with a large amount of oxygen-containing group, can interact with the amino on silicon wafer on GO, from
And GO is firmly adhered on silicon wafer.
In above-mentioned steps 3, the concentration of aqueous solution of chloraurate is not particularly limited, usually in 0.05wt%-2wt%；Absorption
There is AuCl4 -The poly 2 vinyl pyridine brush (P2VP brush) of ion is placed in the closed container containing chromium solution, and the P2VP
Brush is not contacted with pyrroles, and this point is extremely important.Since P2VP brush is not contacted with pyrroles, it is adsorbed with AuCl4 -The P2VP of ion
AuCl in brush4 -Pyrroles's vapor-phase oxidation polymerize by ion obtains polypyrrole, and AuCl4 -Ion itself is reduced into not similar shape
The Au nanostructure 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 used ultraviolet light is 350nm.
In the following, the present invention is more specifically described by following embodiment.Here, embodiment is merely to illustrate the present invention, no
It is construed that limiting the scope of the invention.Implementing the present invention is that can carry out without departing from its spirit and scope
Various changes and modifications.These variations and improvement are within the scope of the appended claims, it should be understood that at being of the invention one
Part.
(embodiment 1)
Step 1: firstly, thering is the silicon wafer of silica dioxide coating to immerse the 3- aminopropyl-triethoxy silicon containing 5% on surface
In the toluene solution of alkane, ultrasonic reaction 2 hours, to obtain amido modified silicon wafer.By 0.025mg/mL graphene oxide
(GO) ethanol solution drips on silica gel seal, and GO is transferred on the silicon wafer with amino using seal stamp transfer method, natural
It is dry, (silicon wafer/GO) of GO modification can be obtained.
Fig. 2 is silicon wafer/GO XPS spectrum, in figure four four peaks of characteristic peak 289.1,287.7,286.6,284.6eV,
They correspond respectively to the carboxyl (COO) of GO, carbonyl (C=O), the C-C/C=C group in epoxy group and aromatic rings, thus
Prove that GO is successfully grafted to silicon chip surface.
Step 2: resulting silicon wafer/GO being dipped into the seal pipe containing 4-vinylpridine monomer, at room temperature with purple
Outer light (wavelength 350nm) is irradiated 2 hours, after reaction, the non-grafted P4VP to the surface GO is removed with chloroform repeated flushing
Polymer obtains silicon wafer/graphene oxide/poly 4 vinyl pyridine brush (silicon wafer/GO/P4VP brush).
Fig. 3 is silicon wafer/GO/P4VP brush XPS figure, the peak apparent N 1s occurs in figure, P4VP is belonged to, to demonstrate,prove
Bright P4VP brush is successfully grafted to the surface GO.
Step 3: by silicon wafer/GO/P4VP brush in gold chloride (HAuCl4) the middle immersion of aqueous solution (1%wt) 12 hours, then
Taking-up is washed with deionized, and removes unadsorbed HAuCl4.HAuCl will be then adsorbed with4Silicon wafer/GO/P4VP brush be placed into
Closed container containing pyrroles, and the silicon wafer/GO/P4VP brush is not contacted with pyrroles, reacts 3 hours to get silicon wafer/oxidation stone is arrived
Black alkene/poly 4 vinyl pyridine brush/polypyrrole-metal/composite material (silicon wafer/GO/P4VP/PPy-Au composite material).
Fig. 4 (A) is silicon wafer/GO/P4VP/PPy-Au composite material SEM figure, it is known that obtains flowers shape Au structure.
Fig. 5 is silicon wafer/GO/P4VP/PPy-Au composite material XPS figure, the apparent peak Au4f is shown in figure, to demonstrate,prove
Bright HAuCl4It has been reduced into Au.
Step 4: silicon wafer/GO/P4VP/PPy-Au composite material being handled 2 hours in 500 DEG C of high temperature anaerobics, in this mistake
P4VP brush and PPy organic matter will be removed in journey, and GO is then changed into rGO, to obtain silicon wafer/rGO/Au composite material.
Fig. 6 (A) is silicon wafer/rGO/Au composite material SEM figure, it can be seen from the figure that although eliminating P4VP and PPy has
Machine object, silicon wafer/rGO/Au pattern are held essentially constant.
(embodiment 2)
Step 1 and step 2 are identical as embodiment.
Step 3: by silicon wafer/GO/P4VP brush in gold chloride (HAuCl4) the middle immersion of aqueous solution (1%wt) 12 hours, then
Taking-up is washed with deionized, and removes unadsorbed HAuCl4.HAuCl will be then adsorbed with4P4VP brush be placed into containing pyrroles
The closed container of solution, and the silicon wafer/GO/P4VP brush is not contacted with chromium solution, reacts 7 hours to get silicon wafer/oxidation stone is arrived
Black alkene/poly 4 vinyl pyridine brush/polypyrrole-metal/composite material (silicon wafer/GO/P4VP/PPy-Au composite material).
Fig. 4 (B) is silicon wafer/GO/P4VP/PPy-Au composite material SEM figure, it is known that obtains coralliform gold nano structure.
Step 4: silicon wafer/GO/P4VP/PPy-Au composite material being handled 2 hours in 500 DEG C of high temperature anaerobics, in this mistake
P4VP brush and PPy organic matter will be removed in journey, and GO is then changed into rGO, to obtain silicon wafer/rGO/Au composite material.
Fig. 6 (B) is silicon wafer/rGO/Au composite material SEM figure, it can be seen from the figure that although eliminating P4VP and PPy has
Machine object, silicon wafer/rGO/Au pattern are held essentially constant.
(reference example)
Silicon wafer/rGO/Au composite material detects 4- aminothiophenol (4-ATP) as Raman substrate
In Raman test process, we select the resulting silicon wafer of embodiment 1/rGO/Au composite material as Raman substrate
Material is prepared the 4-ATP ethanol solution of various concentration first, then rGO/Au composite material is dipped into 4-ATP solution, 6
It as a child took out afterwards, and was washed with deionized 3 times, is finally dried up with the nitrogen stream of high-purity, tested for Raman.Shown in Fig. 7
Various concentration 4-ATP is in silicon wafer/rGO/Au composite material surface Raman spectrum ((a) 10-4M, (b) 10-5M, (c) 10-6M, (d)
10-7M), it can be seen that even if 4-ATP molecular concentration is down to 10-7M, Raman spectrum can still show stronger characteristic peak,
To prove that silicon wafer/rGO/Au composite material is a kind of excellent Raman active substrate material, small organic molecule can be realized
Trace detection.
Claims (2)
1. a kind of preparation method of silicon wafer/reduced graphene/Jenner's nano composite material, including step 1, step 2, step 3 and step
Rapid 4,
Step 1: having the silicon wafer of silica dioxide coating as substrate using surface, by substrate aminofunctional, obtain amido modified silicon
The ethanol solution of graphene oxide is dripped on silica gel seal, is transferred to graphene oxide using seal stamp transfer method by piece
On the amido modified silicon wafer, the silicon wafer of graphene oxide modification is obtained；
Step 2: the silicon wafer that resulting graphene oxide is modified being dipped into the seal pipe containing 4-vinylpridine monomer, is used
Ultraviolet light 30-180min takes out silicon wafer and rinsed with chloroformic solution after reaction, obtains silicon wafer/graphene oxide/poly-
4-vinylpridine brush；
Step 3: resulting silicon wafer/graphene oxide/poly 4 vinyl pyridine brush being immersed in aqueous solution of chloraurate, when immersion
Between be 6-18h, after taking-up, be washed with deionized, obtain being adsorbed with AuCl4 -Silicon wafer/graphene oxide of ion/poly- 4- ethylene
Yl pyridines brush, then resulting silicon wafer/graphene oxide/poly 4 vinyl pyridine brush is placed on the closed container containing pyrroles
In, and the silicon wafer/graphene oxide/poly 4 vinyl pyridine brush is not contacted with pyrroles, reacts 1-8h, silicon wafer/oxygen can be obtained
Graphite alkene/poly 4 vinyl pyridine brush/polypyrrole-metal/composite material；
Step 4: by resulting silicon wafer/graphene oxide/poly 4 vinyl pyridine brush/polypyrrole-metal/composite material in 400-800
DEG C, anaerobic handles 0.5-3h, obtains silicon wafer/reduced graphene/metal/composite material.
2. the preparation method of silicon wafer/reduced graphene/Jenner's nano composite material according to claim 1, the substrate
Aminofunctional is obtained by the way that substrate to be dipped into amino-containing silane coupler solution.
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| CN110514640B (en) * | 2019-08-01 | 2022-07-01 | 中国科学院合肥物质科学研究院 | Surface enhanced Raman spectroscopy detection technology based on inorganic sensitive layer and material preparation thereof |
| 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 |
| CN112387981A (en) * | 2020-10-26 | 2021-02-23 | 东莞职业技术学院 | Graphene nanoparticle composite material with high conductivity and preparation method thereof |
| CN112708402B (en) * | 2020-12-29 | 2022-03-15 | 广东省科学院化工研究所 | Preparation method of high-thermal-conductivity graphene composite material |
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