CN105149613A - Preparation method for flaky silver nanometer materials - Google Patents
Preparation method for flaky silver nanometer materials Download PDFInfo
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- CN105149613A CN105149613A CN201510616658.XA CN201510616658A CN105149613A CN 105149613 A CN105149613 A CN 105149613A CN 201510616658 A CN201510616658 A CN 201510616658A CN 105149613 A CN105149613 A CN 105149613A
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Abstract
The invention discloses a preparation method for flaky silver nanometer materials. The method includes the following steps that firstly, at the existence of sodium citrate, a sodium borohydride solution prepared through ice water is used for reducing silver nitrate so that a silver seed solution is formed; secondly, a p-dihydroxybenzene solution, a sodium citrate buffer solution, the silver seed solution, a DNA solution, water and a silver nitrate solution are measured and taken according to the volume ratio of 3-5:3-5:1-3:1-3:27-30:9-12; and thirdly, after the p-dihydroxybenzene solution, the sodium citrate buffer solution, the silver seed solution, the DNA solution and the water are fully mixed, the silver nitrate solution is added, the mixture is kept away from light and grows for 12-14 h at the temperature of 20-24 DEG C, and then the flaky silver nanometer materials can be obtained. Compared with a traditional method, the preparation method is good in biocompatibility and high in universality, and a new platform is provided for application of the flaky silver nanometer materials in biological analysis and biomedicine.
Description
Technical field
The invention belongs to silver nano material technical field, be specifically related to a kind of preparation method of sheet silver nano material.
Background technology
The shape of silver nano material plays decisive role, comprising surface plasmon resonance effect and surface enhanced Raman scattering effect for its physicochemical properties.(El-Sayed, M.A.SomeInterestingPropertiesofMetalsConfinedinTimeandNa nometerSpaceofDifferentShapes [J] .Acc.Chem.Res.2001,34,257-264; Nie, S.; Emory, S.R.ProbingSingleMoleculesandSingleNanoparticlesbySurfac e-EnhancedRamanScattering [J] .Science1997,275,1102-1106) difformity silver nano material can be synthesized by the method for seed anisotropic growth, therefore, it is possible to controlled adjustment optics and electrology characteristic.Silver nano material is widely used in the middle of bioanalysis and biomedicine due to these good characteristics.At present, can synthesize various shape silver nano-grain, as spherical, cube, octahedron, sheet, bar-shaped and linear.(Sun, Y.; Xia, Y.Shape-ControlledSynthesisofGoldandSilverNanoparticles [J] .Science2002,298,2176-2179; Jin, R.; Cao, Y.; Mirkin, C.A.; Kelly, K.L.; Schatz, G.C.; Zheng, J.G.PhotoinducedConversionofSilverNanospherestoNanoprism s [J] .Science2001,294,1901-1903; Rycenga, M.; Cobley, C.M.; Zeng, J.; Li, W.; Moran, C.H.; Zhang, Q.; Qin, D.; Xia, Y.ControllingtheSynthesisandAssemblyofSilverNanostructur esforPlasmonicApplications [J] .Chem.Rev.2011,111, but 3669-3712) synthesize these silver nanoparticles to need to use cetyl ammonium bromide, (Chen, S.; Carroll, D.L.SynthesisandCharacterizationofTruncatedTriangularSil verNanoplates [J] .NanoLett.2002,2,1003-1007) oleyl amine, (Yener, D.O.; Sindel, J.; Randall, C.A.; Adair, J.H.SynthesisofNanosizedSilverPlateletsinOctylamine-Wate rBilayerSystems [J] .Langmuir2002,18,8692-8699) N, N '-dimethyl formamide, (Pastoriza-Santos, I.; Liz-Marz á n, L.M.SynthesisofSilverNanoprismsinDmf [J] .NanoLett.2002,2,903-905) polyvinylpyrrolidone (MachulekJunior, A.; MoisesdeOliveira, H.P.; Gehlen, M.H.PreparationofSilverNanoprismsUsingPoly (N-Vinyl-2-Pyrrolidone) asaColloid-StabilizingAgentandtheEffectofSilverNanoparti clesonthePhotophysicalPropertiesofCationicDyes.Photochem [J] .Photobiol.Sci.2003,2,921-925) etc. with the part of silver nano material particular crystal plane strong interaction.But the shape bio-toxicity that these parts well can regulate and control silver nano material is comparatively strong, limits the application of silver nano material in bioanalysis and biomedicine.Therefore, the silver nano material developing the method synthesis given shape of good biocompatibility has great importance.
Summary of the invention
The object of the invention is to overcome prior art defect, a kind of preparation method of sheet silver nano material is provided.
Concrete technical scheme of the present invention is as follows:
A preparation method for sheet silver nano material, comprises the steps:
(1) under natrium citricum exists, the sodium borohydride solution reduction silver nitrate utilizing frozen water to prepare, forms silver-colored seed solution;
(2) measure biphenol solution by the volume ratio of 3 ~ 5:3 ~ 5:1 ~ 3:1 ~ 3:27 ~ 30:9 ~ 12, sodium citrate buffer solution, above-mentioned silver-colored seed solution, DNA solution, water and liquor argenti nitratis ophthalmicus, be wherein 0.133 ~ 3.33mM to the concentration of biphenol solution, the concentration of sodium citrate buffer solution is 20 ~ 500mM, pH is 1.5 ~ 5.5, the concentration of liquor argenti nitratis ophthalmicus is 0.133 ~ 3.33mM, the concentration of DNA solution is 20.7 ~ 332 μMs, DNA is wherein the oligodeoxynucleotide fragment of same deoxynucleotide composition, length is 12 ~ 40bp, the mass ratio of silver seed and DNA is 1.6 ~ 6.4:100,
(3) after the sodium citrate buffer solution to biphenol solution, pH1.5 ~ 5.5, above-mentioned silver-colored seed solution, DNA solution and water fully being mixed, add liquor argenti nitratis ophthalmicus, at 20 ~ 24 DEG C, lucifuge growth 12 ~ 14h, obtains described sheet silver nano material.
In a preferred embodiment of the invention, the described volume ratio to biphenol solution, sodium citrate buffer solution, above-mentioned silver-colored seed solution, DNA solution, water and liquor argenti nitratis ophthalmicus is 4:4:2:2:28:10.
Preferred further, the described concentration to biphenol solution is 0.333 ~ 1.332mM.
Preferred further, the pH of described sodium citrate buffer solution is 3 ~ 4, and concentration is 50 ~ 100mM.
Preferred further, the concentration of described DNA solution is 41.5 ~ 166 μMs.
Preferred further, described deoxynucleotide comprises adenylic acid, guanylic acid, cytidylic acid and thymidylic acid.
Preferred further, the length of described DNA is 12bp.
Preferred further, the concentration of described liquor argenti nitratis ophthalmicus is 0.333 ~ 1.332mM.
Preferred further, the temperature of described step (3) is 22 DEG C.
The invention has the beneficial effects as follows:
1, the part that the DNA that preparation method of the present invention have chosen good biocompatibility grows as silver nano material, makes the silver nano material synthesized have good biocompatibility;
2, preparation method of the present invention utilizes the strong interaction of DNA and silver nanoparticle particular crystal plane to regulate and control the silver nano material of synthesizing flaky structure;
3, preparation method of the present invention utilizes not homotactic DNA different with interaction mode from silver nano-grain interaction strength, the difform sheet silver nano material of regulation and control synthesis;
4, the whole process that preparation method of the present invention synthesizes silver nano material is carried out all in aqueous, avoids using polyalcohol, N, the organic solvents such as N '-dimethyl formamide;
5, preparation method of the present invention is compared with conventional method, and this method Bc is good, highly versatile, for sheet silver nano material provides new platform in bioanalysis and biomedical application.
Accompanying drawing explanation
Fig. 1 is the composition principle figure of sheet silver nano material of the present invention.
Fig. 2 is scanning electron microscope (SEM) photograph (A) and the domain size distribution statistical chart (B) of the silver-colored seed of sodium borohydride reduction synthesis in the step (1) of the embodiment of the present invention 1.
The uv-visible absorption spectra of the silver-colored seed that in Fig. 3, (A) is prepared for the embodiment of the present invention 1 step (1) and the obtained sheet silver nano material of embodiment 1; (B) be scanning electron microscope (SEM) photograph and the transmission electron microscope picture of the obtained triangle sheet silver nano-grain of the embodiment of the present invention 1; (C) be the high-resolution-ration transmission electric-lens figure of the obtained triangle sheet silver nanoparticle of the embodiment of the present invention 1; (D) be the SEAD figure of the obtained triangle sheet silver nanoparticle of the embodiment of the present invention 1.
Fig. 4 (A) is grain weight synthesis triangle sheet silver nano-grain different in the present invention; (B) be the 250 μMs of C12DNA synthesizing flaky silver nano-grains of different volumes in the present invention.
Fig. 5 (A) is the length of side statistical chart of the present invention's different grain weight synthesis triangle sheet silver nano-grain; (B) be the length of side statistical chart of different volumes of the present invention 250 μMs of C12DNA synthesizing flaky silver nano-grains.
Fig. 6 (A) is the scanning electron microscope (SEM) photograph of different temperatures synthesizing flaky silver nano-grain of the present invention; (B) be the length of side statistical chart of different temperatures synthesizing flaky silver nano-grain of the present invention; (C) be the schematic diagram of the different sequence DNA of the present invention (12bp length, is made up of completely respectively T, A and G, is designated as A12, T12 and G12) mediation synthesis difformity silver nano-grain.
Fig. 7 (A) is the scanning electron microscope (SEM) photograph of the present invention's different sequence DNA synthesizing flaky silver nano-grain; (B) be the scanning electron microscope (SEM) photograph of different length C base DNA synthesizing flaky silver nano-grain of the present invention.
Fig. 8 be the x-ray photoelectron power spectrum phenogram (A) of silver element on the sheet silver nano material of the obtained DNA mediation synthesis of the embodiment of the present invention 1 and DNA and silver nano material interactional x-ray photoelectron power spectrum phenogram (B).
Detailed description of the invention
By reference to the accompanying drawings below by way of detailed description of the invention technical scheme of the present invention is further detailed and is described.
Embodiment 1
As shown in Figure 1, specific experiment condition gropes process as shown in Figures 4 to 7 to the technology path of the present embodiment, and concrete steps are as follows:
(1) synthesis of silver-colored seed is undertaken (as Fig. 1) by sodium borohydride reduction, 0.7mL water, 25 μ L10mM silver nitrates, 25 μ L10mM natrium citricums are added successively in 1.5mL centrifuge tube, the sodium borohydride aqueous solution of 300 μ L1mM frozen water preparations is added after mixing, thermal agitation 20s, room temperature obtains silver-colored seed solution after placing and within 2 hours, waiting for that sodium borohydride decomposes.Silver-colored seed after synthesis as shown in Figure 2.
(2) synthesis of sheet silver nano material is undertaken by the mode of seed growth.Building-up process is in 200 μ L centrifuge tubes, add 4 μ L10mM hydroquinones, the sodium citrate buffer solution of 4 μ L100mMpH3.5,2 μ L synthetic silver-colored seed solution, 2 μ L250 μM DNA (C12---12bp length successively, all be made up of C), 28 μ L water, add 20 μ L2mM silver nitrates by after above-mentioned solution mixing, under the condition of 22 DEG C of lucifuges, grow 12h synthesizing flaky silver nano-grain.Characterize synthetic sheet silver nano material by ultraviolet-visible spectrum, ESEM, transmission electron microscope and x-ray photoelectron power spectrum, result is as shown in Fig. 2 to Fig. 8.
Those of ordinary skill in the art are known, when composition of the present invention and parameter change in following ranges, still can obtain same as the previously described embodiments or close technique effect, all belong to protection scope of the present invention:
A preparation method for sheet silver nano material, comprises the steps:
(1) under natrium citricum exists, the sodium borohydride solution reduction silver nitrate utilizing frozen water to prepare, forms silver-colored seed solution;
(2) measure biphenol solution by the volume ratio (preferred 4:4:2:2:28:10) of 3 ~ 5:3 ~ 5:1 ~ 3:1 ~ 3:27 ~ 30:9 ~ 12, sodium citrate buffer solution, above-mentioned silver-colored seed solution, DNA solution, water and liquor argenti nitratis ophthalmicus, be wherein 0.133 ~ 3.33mM (preferably 0.333 ~ 1.332mM) to the concentration of biphenol solution, the concentration of sodium citrate buffer solution is 20 ~ 500mM, pH is 1.5 ~ 5.5 (preferably 50 ~ 100mM, pH is 3 ~ 4), the concentration of liquor argenti nitratis ophthalmicus is 0.133 ~ 3.33mM (0.333 ~ 1.332mM), the concentration of DNA solution is 20.7 ~ 332 μMs, DNA is wherein the oligodeoxynucleotide fragment of same deoxynucleotide composition, length is that 12 ~ 40bp is (preferred, the concentration of described DNA solution is 41.5 ~ 166 μMs, described deoxynucleotide comprises adenylic acid (A), guanylic acid (G), cytidylic acid (C) and thymidylic acid (T)), the mass ratio of silver seed and DNA is 1.6 ~ 6.4:100,
(3) after the sodium citrate buffer solution to biphenol solution, pH1.5 ~ 5.5, above-mentioned silver-colored seed solution, DNA solution and water fully being mixed, add liquor argenti nitratis ophthalmicus, at 20 ~ 24 DEG C, lucifuge growth 12 ~ 14h, obtains described sheet silver nano material.
The above, be only preferred embodiment of the present invention, therefore can not limit scope of the invention process according to this, the equivalence change namely done according to the scope of the claims of the present invention and description with modify, all should still belong in scope that the present invention contains.
Claims (9)
1. a preparation method for sheet silver nano material, is characterized in that: comprise the steps:
(1) under natrium citricum exists, the sodium borohydride solution reduction silver nitrate utilizing frozen water to prepare, forms silver-colored seed solution;
(2) measure biphenol solution by the volume ratio of 3 ~ 5:3 ~ 5:1 ~ 3:1 ~ 3:27 ~ 30:9 ~ 12, sodium citrate buffer solution, above-mentioned silver-colored seed solution, DNA solution, water and liquor argenti nitratis ophthalmicus, be wherein 0.133 ~ 3.33mM to the concentration of biphenol solution, the concentration of sodium citrate buffer solution is 20 ~ 500mM, pH is 1.5 ~ 5.5, the concentration of liquor argenti nitratis ophthalmicus is 0.133 ~ 3.33mM, the concentration of DNA solution is 20.7 ~ 332 μMs, DNA is wherein the oligodeoxynucleotide fragment of same deoxynucleotide composition, length is 12 ~ 40bp, the mass ratio of silver seed and DNA is 1.6 ~ 6.4:100,
(3) after the sodium citrate buffer solution to biphenol solution, pH1.5 ~ 5.5, above-mentioned silver-colored seed solution, DNA solution and water fully being mixed, add liquor argenti nitratis ophthalmicus, at 20 ~ 24 DEG C, lucifuge growth 12 ~ 14h, obtains described sheet silver nano material.
2. the preparation method of a kind of sheet silver nano material as claimed in claim 1, is characterized in that: the described volume ratio to biphenol solution, sodium citrate buffer solution, above-mentioned silver-colored seed solution, DNA solution, water and liquor argenti nitratis ophthalmicus is 4:4:2:2:28:10.
3. the preparation method of a kind of sheet silver nano material as claimed in claim 1 or 2, is characterized in that: the described concentration to biphenol solution is 0.333 ~ 1.332mM.
4. the preparation method of a kind of sheet silver nano material as claimed in claim 1 or 2, is characterized in that: the pH of described sodium citrate buffer solution is 3 ~ 4, and concentration is 50 ~ 100mM.
5. the preparation method of a kind of sheet silver nano material as claimed in claim 1 or 2, is characterized in that: the concentration of described DNA solution is 41.5 ~ 166 μMs.
6. the preparation method of a kind of sheet silver nano material as claimed in claim 1 or 2, is characterized in that: described deoxynucleotide comprises adenylic acid, guanylic acid, cytidylic acid and thymidylic acid.
7. the preparation method of a kind of sheet silver nano material as claimed in claim 1 or 2, is characterized in that: the length of described DNA is 12bp.
8. the preparation method of a kind of sheet silver nano material as claimed in claim 1 or 2, is characterized in that: the concentration of described liquor argenti nitratis ophthalmicus is 0.333 ~ 1.332mM.
9. the preparation method of a kind of sheet silver nano material as claimed in claim 1 or 2, is characterized in that: the temperature of described step (3) is 22 DEG C.
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Cited By (4)
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| CN106601914A (en) * | 2016-12-22 | 2017-04-26 | 东南大学 | Method for preparing polycrystalline ultra-thin metal film and two-dimensional nano pattern |
| CN107486563A (en) * | 2017-09-05 | 2017-12-19 | 中南大学 | A kind of method for improving Nano silver grain antibacterial activity |
| CN110449188A (en) * | 2019-08-15 | 2019-11-15 | 苏州大学 | Silver citrate/silver composite nano materials and its preparation method and application |
| CN114042929A (en) * | 2021-10-26 | 2022-02-15 | 西安交通大学 | High-concentration silver nano-micron sheet and synthesis method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106601914A (en) * | 2016-12-22 | 2017-04-26 | 东南大学 | Method for preparing polycrystalline ultra-thin metal film and two-dimensional nano pattern |
| CN107486563A (en) * | 2017-09-05 | 2017-12-19 | 中南大学 | A kind of method for improving Nano silver grain antibacterial activity |
| CN110449188A (en) * | 2019-08-15 | 2019-11-15 | 苏州大学 | Silver citrate/silver composite nano materials and its preparation method and application |
| CN114042929A (en) * | 2021-10-26 | 2022-02-15 | 西安交通大学 | High-concentration silver nano-micron sheet and synthesis method thereof |
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