CN105562682A - Graphene-wrapped gold nanorod composite nanomaterial and preparation method thereof - Google Patents
Graphene-wrapped gold nanorod composite nanomaterial and preparation method thereof Download PDFInfo
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- CN105562682A CN105562682A CN201610024662.1A CN201610024662A CN105562682A CN 105562682 A CN105562682 A CN 105562682A CN 201610024662 A CN201610024662 A CN 201610024662A CN 105562682 A CN105562682 A CN 105562682A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a graphene-wrapped gold nanorod composite nanomaterial of a core-shell structure. A gold nanorod is used as the core, graphene is used as the shell, the thickness of graphene is 1-2 nm, and the mass of graphene accounts for 0.005-0.05% of the mass of the composite nanomaterial. The graphene-wrapped gold nanorod composite nanomaterial is large in Raman enhancement of graphene, and wide in application range.
Description
Technical field
The present invention relates to a kind of Graphene trapping gold nanometer rods composite nano materials and preparation method thereof.
Background technology
Carbon nanomaterial causes the extensive concern of people due to the physicochemical property of its uniqueness.Along with the industrialization of carbon nanomaterial, various forms of carbon nanomaterial enters the life of people in different forms, and grapheme material is exactly one of them.Grapheme material, except having the feature of two-photon and physics thermotherapy, can also be applied to Raman detection and Raman image according to the Raman trait of Graphene.SERS (surface-enhancedRamanscattering, SERS) can make the Molecular Raman signal being adsorbed on surface amplify about 10
6~ 10
14doubly, sensitivity improves greatly.Therefore in Graphene metal Raman substrate in addition, the Raman signal of Graphene can be made to improve greatly.
CN201310729507.6 discloses a kind of preparation method of gold-graphene composite nano material, it is by CVD method synthesizing graphite alkene parcel gold goal nano material, its core is spherical, the intensity of the surface plasma body resonant vibration of gold goal is not strong, it is in thermotherapy, two-photon, and the enhancing degree aspect of graphite Raman is all had much room for improvement.
Summary of the invention
The technical problem that the present invention solves is, improves gold further and strengthens degree to the Raman of Graphene, make the application of gold-graphene composite Nano ion more extensive.
Technical scheme of the present invention is, a kind of Graphene trapping gold nanometer rods composite nano materials is provided, described Graphene trapping gold nanometer rods composite nano materials is nucleocapsid structure, take gold nanorods as core, Graphene is shell, the thickness of Graphene is 1-2nm, and the quality of Graphene accounts for 0.005-0.05% of described composite nano materials quality.
Further, the length 58-65nm of gold nanorods, wide 10-15nm.
The present invention further provides a kind of preparation method of Graphene trapping gold nanometer rods composite nano materials, comprise the following steps:
(1) in 1 parts by volume concentration be 1.7-2.5g/L coated with silica gold nanorods solution in add the methyl alcohol of 3-8 parts by volume, ultrasonic, obtain solution C;
SiO is added in methyl alcohol
2powder, ultrasonic, obtain solution D, SiO in solution D
2the mass volume ratio of powder and methyl alcohol is 1:75-85, and mass unit is g, and volume unit is mL;
Carry out ultrasonic after the solution C of 1-1.5 parts by volume is mixed with the solution D of 1 parts by volume, then remove methyl alcohol, the mixture obtained is dried to obtain solids;
(2) by the solids grind into powder of step (1), at CH
4flow is 20-100cm
2calcination 10-18min under the flow conditions of/mL, the temperature of calcination is 800-1000 DEG C; Cool after calcination, then mix with the mixed solution that HF, second alcohol and water form and remove silica, centrifugal, obtain Graphene trapping gold nanometer rods composite nanometer particle after isolating centrifugate; In the mixed solution of described HF, second alcohol and water composition, the volume ratio of HF, second alcohol and water is 1.8-2.2:1:1; The mass volume ratio of the mixed solution that described powder and HF, second alcohol and water form is 1.25-1.35:6-8, and mass unit is g, and volume unit is mL.
Further, described SiO
2the particle diameter of powder is 5-40nm.
Further, described ultrasonic power is 170-210W, and ultrasonic time is 1-2h.
Further, in step (1), the preparation method of coated with silica gold nanorods solution is as follows: in gold nanorods solution, add ethyl orthosilicate, stir, reacted rear centrifugal, the solid after centrifugal is dissolved in methyl alcohol and obtains described coated with silica gold nanorods solution.
Further, Graphene trapping gold nanometer rods composite nano materials step (2) obtained mixes containing the Aqueous Solutions of Polyethylene Glycol of alkyl with 15-25mg/mL, ultrasonic to dissolving, and obtains Graphene trapping gold nanometer rods composite nano materials solution; Graphene trapping gold nanometer rods composite nano materials is 2.8-3.2:3 with the mass volume ratio of the Aqueous Solutions of Polyethylene Glycol containing alkyl, and mass unit is mg, and volume unit is mL.
Further, the described polyethylene glycol containing alkyl is C
18-PEG, C
18-PEG represents that the alkyl chain be connected with PEG be carbon number is 18.
Graphene trapping gold nanometer rods composite nano materials (hereinafter referred to as " AuNRG nano material ") is that (AuNR represents gold nanorods to a kind of inorganic composite materials, represent parcel or coated, G represents Graphene), make to wrap up a few layer graphene around gold nanorods by the method for CVD, it is well applied in biochemistry detection and bio-imaging.AuNRG nano material is because of the protection of the Graphene of its appearance, and its stability is fine, can place the several months in atmosphere.AuNRG nano material also can be used as a kind of Raman enhancing substrate and detects some Raman signal molecules.Itself also there is unique Raman scattering character, can be used for SERS Raman image.AuNRG nano material also has strong two-photon fluorescence, can be used as another mode for cell imaging.Utilize the character of the specific binding of aptamer and Graphene, modify on the surface of AuNRG, target is carried out to tissue, for two-photon and Raman image.
This is that first time is at the surface of gold nanorods parcel Graphene.Gold nanorods is at high temperature easily deformed into spherical, therefore carries out SiO at pretreatment process
2parcel, make AuNR at high temperature keep its form.AuNRG has possessed the double properties of Graphene and gold nanorods, has excellent physico-chemical property.And the method is simple, operate controlled.
The intensity of the surface plasma body resonant vibration of gold goal is not strong, at high temperature easily obtains, but core is gold nano, and bar-shaped graphene nano material is at high temperature not easy preparation.The present invention is by carrying out SiO to gold nanorods
2parcel still ensure bar-shaped maintenance when making it at high temperature carry out the process of CVD.Obtained its Raman to Graphene of Graphene trapping gold nanometer rods nano material strengthens larger, and its application is more extensive.
Beneficial effect of the present invention is: this preparation method is simple, and cost is low, and controllability is strong.The AuNRG composite nano materials homogeneity prepared is good, stable in properties.And this nano material has multiple character, as two-photon fluorescence, Raman signal, SERS substrate, near infrared absorption etc.This is that first time is at the surface of gold nanorods parcel Graphene.Gold nanorods is at high temperature easily deformed into spherical, therefore carries out SiO at pretreatment process
2parcel, make AuNR at high temperature keep its form.AuNRG has possessed the double properties of Graphene and gold nanorods, has excellent physico-chemical property.And the method is simple, operate controlled.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of AuNRG nano particle prepared by the present invention; Wherein, a) being particle schematic diagram, b) is high resolution electron microscopy figure, the c of particle) be AuNRSiO
2transmission electron microscope picture, d) be the ultrahigh resolution Electronic Speculum figure of particle;
Fig. 2 be the Raman spectrogram of AuNRG particle prepared by the present invention a), the Raman enhanced spectrum figure b of R6G) and cell Raman image figure c);
Fig. 3 is that AuNRG and AuG of the present invention compares the enhancing signal of Graphene under 633nm laser;
Fig. 4 is the two-photon fluorescence cell imaging figure of AuNRG nano particle of the present invention;
Fig. 5 be AuNRG of the present invention carry out aptamer modified after imaging of tissue; A) for particle is at the Raman image of cancerous tissue and normal structure; B) for particle is in the two-photon imaging of cancerous tissue and normal structure.
Detailed description of the invention
Embodiment 1
Preparation method's step of Graphene trapping gold nanometer rods composite nano materials is as follows:
(1) by the chlorauric acid solution of 0.25mL0.01mol/L, join in the CTAB solution of 9.75mL0.1mol/L, mix.Then 0.6mL0.01mol/L sodium borohydride solution freshly prepared in ice-water bath is added rapidly in above-mentioned mixed liquor, quick reversing 2min, then at room temperature 2h is left standstill, obtain solution A. the liquor argenti nitratis ophthalmicus of 1mL0.01mol/L is added in the chlorauric acid solution of 5mL0.01mol/L, add the CTAB solution of 100mL0.1mol/L again, mix.Then in above-mentioned solution, the hydrochloric acid of 2mL1mol/L and the AA(ascorbic acid of freshly prepared 0.8mL0.1mol/L is added successively).Finally by gained mixed liquor reversing mixing, obtain solution B.Add in solution B 0.25mL leave standstill 2h after solution A, reversing mixing 10s, then at room temperature leave standstill more than 6h namely obtain gold nanorods solution.
(2) the gold nanorods solution of step (1) gained is carried out twice centrifugal, centrifugal rotational speed is 11000rpm, and the time is 25min.Centrifugal rear removal supernatant liquor, lower floor is dissolved in ultra-pure water, and with 0.1MCTAB, the concentration of CTAB in solution is adjusted to 0.8mM.In 10mL gold nanorods solution, add 40 μ L0.1mol/LNaOH its pH is adjusted to 10.6, after stirring 30min, add 90 μ L20%TEOS (being dissolved in methyl alcohol) wherein and be placed in 30 DEG C and stir 20h.Then, under the centrifugal condition of 10000rpm, 20min, remove supernatant liquor, lower floor is dissolved in 2mL methyl alcohol, obtains AuNRSiO
2solution.
(3) by the AuNRSiO of step (2) gained
2solution adds ultrasonic 1-2h in methyl alcohol, obtains solution C, by SiO
2add ultrasonic process 1-2h in another part of methyl alcohol, obtain solution D, SiO
2dividing with the mass volume ratio of methyl alcohol is 1:75-85, and mass unit is g, and volume unit is mL; Carry out ultrasonic process 1-2h again after mixed C solution and solution D, removing methyl alcohol, dries the mixture obtained under 75-85 DEG C of conditions; Ultrasonic wave process described in step (3) refers to ultrasonic process under 170-190w condition;
(4) by the mixed grinding powdered of step (3) gained, then in CH
4flow is 50cm
2calcination 15min under the flow conditions of/mL, calcination temperature is 800-1000 DEG C, mixes after cooling with the mixed solution that HF, second alcohol and water form, centrifugal, obtains AuNRG nano particle after being separated centrifugate; Wherein, described HF, second alcohol and water composition mixed solution in HF, second alcohol and water volume ratio be 1.8-2.2:1:1; The mass volume ratio of the mixed solution that described powder and HF, second alcohol and water form is 1.25-1.35:6-8, and mass unit is g, and volume unit is mL.
Fig. 1-5 is the test phenogram to the obtained composite nano materials of embodiment 1, and Fig. 1 is the transmission electron microscope picture of AuNRG nano particle prepared by the present invention; Wherein, a) being particle schematic diagram, b) is high resolution electron microscopy figure, the c of particle) be AuNRSiO
2transmission electron microscope picture, d) be the ultrahigh resolution Electronic Speculum figure of particle; Can show that AuNRG is nucleocapsid structure, core is gold nanorods long 58-65nm, wide 10-15nm, and a few layer graphene that has of shell is about 1-1.5nm, and as calculated, the quality of Graphene accounts for 0.02% of described composite nano materials quality.
Fig. 2 be the Raman spectrogram of AuNRG particle prepared by the present invention a), the Raman enhanced spectrum figure b of R6G) and cell Raman image figure c).Fig. 3 is that AuNRG and AuG of the present invention compares the Raman enhancing signal of Graphene under 633nm laser, and the Raman signal of the enhancing Graphene of AuNRG will double than AuG, AuG and Graphene trapping gold nanoparticle, i.e. structure disclosed in CN201310729507.6.
Fig. 4 is the two-photon fluorescence cell imaging figure of AuNRG nano particle of the present invention.Fig. 5 be AuNRG of the present invention carry out aptamer modified after imaging of tissue; A) for particle is at the Raman image of cancerous tissue and normal structure; B) for particle is in the two-photon imaging of cancerous tissue and normal structure.
To sum up, this invention synthesized by Graphene trapping gold nanometer rods composite nano materials have the following advantages: 1, preparation method is simple, easy to operate, good properties; 2, AuNRG nano material is also that a kind of Raman strengthens substrate, can detect some Raman signal molecules; 3, AuNRG nano material is not only according to there being Raman character also to have the character of two-photon, may be used for Raman and two-photon multi-modal become; 4, aptamer modified AuNRG nano particle has targeting for cancerous tissue.5, compared with AuG, it will be twice left and right to the enhancing of the Raman signal of Graphene.
Embodiment 2
For improving the water-soluble of this AuNRG composite nanometer particle, AuNRG composite nanometer particle embodiment obtained carries out modification, and step is as follows: AuNRG composite nanometer particle and concentration are the C of 20mg/mL
18-PEG the aqueous solution is pressed mass volume ratio 1:1 and is mixed, and mass unit is mg, and volume unit is mL, and under 190-210W condition, ultrasonic process 2-4 hours, dissolves completely to particle, obtains gold-graphene composite nano material solution.
Claims (8)
1. a Graphene trapping gold nanometer rods composite nano materials, it is characterized in that, described Graphene trapping gold nanometer rods composite nano materials is nucleocapsid structure, take gold nanorods as core, Graphene is shell, the thickness of Graphene is 1-2nm, and the quality of Graphene accounts for 0.005-0.05% of described composite nano materials quality.
2. composite nano materials as claimed in claim 1, is characterized in that, the length 58-65nm of gold nanorods, wide 10-15nm.
3. a preparation method for Graphene trapping gold nanometer rods composite nano materials, is characterized in that, comprise the following steps:
(1) in 1 parts by volume concentration be 1.7-2.5g/L coated with silica gold nanorods solution in add the methyl alcohol of 3-8 parts by volume, ultrasonic, obtain solution C;
SiO is added in methyl alcohol
2powder, ultrasonic, obtain solution D, SiO in solution D
2the mass volume ratio of powder and methyl alcohol is 1:75-85, and mass unit is g, and volume unit is mL;
Carry out ultrasonic after the solution C of 1-1.5 parts by volume is mixed with the solution D of 1 parts by volume, then remove methyl alcohol, the mixture obtained is dried to obtain solids;
(2) by the solids grind into powder of step (1), at CH
4flow is 20-100cm
2calcination 10-18min under the flow conditions of/mL, the temperature of calcination is 800-1000 DEG C; Cool after calcination, then mix with the mixed solution that HF, second alcohol and water form and remove silica, centrifugal, obtain Graphene trapping gold nanometer rods composite nanometer particle after isolating centrifugate; In the mixed solution of described HF, second alcohol and water composition, the volume ratio of HF, second alcohol and water is 1.8-2.2:1:1; The mass volume ratio of the mixed solution that described powder and HF, second alcohol and water form is 1.25-1.35:6-8, and mass unit is g, and volume unit is mL.
4. preparation method as claimed in claim 3, is characterized in that, described SiO
2the particle diameter of powder is 5-40nm.
5. preparation method as claimed in claim 3, it is characterized in that, described ultrasonic power is 170-210W, and ultrasonic time is 1-2h.
6. preparation method as claimed in claim 3, it is characterized in that, in step (1), the preparation method of coated with silica gold nanorods solution is as follows: in gold nanorods solution, add ethyl orthosilicate, stir, reacted rear centrifugal, the solid after centrifugal is dissolved in methyl alcohol and obtains described coated with silica gold nanorods solution.
7. preparation method as claimed in claim 3, it is characterized in that, Graphene trapping gold nanometer rods composite nano materials step (2) obtained mixes containing the Aqueous Solutions of Polyethylene Glycol of alkyl with 15-25mg/mL, ultrasonic to dissolving, obtain Graphene trapping gold nanometer rods composite nano materials solution; Graphene trapping gold nanometer rods composite nano materials is 2.8-3.2:3 with the mass volume ratio of the Aqueous Solutions of Polyethylene Glycol containing alkyl, and mass unit is mg, and volume unit is mL.
8. preparation method as claimed in claim 7, is characterized in that, the described polyethylene glycol containing alkyl is C
18-PEG.
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Cited By (2)
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| CN106944615A (en) * | 2017-05-11 | 2017-07-14 | 洛阳理工学院 | A kind of preparation method of solid coated with silica gold nanorods composite nano materials |
| CN107189314A (en) * | 2017-05-17 | 2017-09-22 | 宁波大学 | A kind of gold/polymer/gold three-layer nuclear shell nanometer dumbbell material and its preparation method and application |
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| CN107189314A (en) * | 2017-05-17 | 2017-09-22 | 宁波大学 | A kind of gold/polymer/gold three-layer nuclear shell nanometer dumbbell material and its preparation method and application |
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