CN105014094A - Core-shell-structure silver-gold nanosheet based on epitaxial growth and preparation method and application thereof - Google Patents
Core-shell-structure silver-gold nanosheet based on epitaxial growth and preparation method and application thereof Download PDFInfo
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- CN105014094A CN105014094A CN201510424180.0A CN201510424180A CN105014094A CN 105014094 A CN105014094 A CN 105014094A CN 201510424180 A CN201510424180 A CN 201510424180A CN 105014094 A CN105014094 A CN 105014094A
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Abstract
The invention provides a core-shell-structure silver-gold nanosheet based on epitaxial growth and a preparation method and application thereof. The method includes the steps that firstly, a silver nanosheet solution is prepared, then, chloroauric acid and ligand react in the alkaline environment, and a gold precursor solution is obtained; and a reducing agent, surfactant, a pH modifier, ligand or acetonitrile and the silver nanosheet solution are added to the gold precursor solution, and the core-shell-structure silver-gold nanosheet is obtained after the reaction. The ligand and chloroauric acid radial can generate coordination, a gold precursor is formed, the redox potential of gold is reduced, and the replacement reaction is prevented from being generated; the gold precursor is reduced into gold atoms through the reducing agent, the gold atoms are deposited on the surface layer of a silver nanosheet in an epitaxial growth mode, and the core-shell-structure silver-gold nanosheet is formed. The preparation process is simple and feasible; the shape and the size of the core-shell-structure silver-gold nanosheet are controllable; the excellent stability and the good optical property are achieved; wide application prospects are achieved in the fields of molecular detection and the like.
Description
Technical field
The invention belongs to technical field of nano material, particularly a kind of silver-gold-nano-piece based on epitaxially grown nucleocapsid structure and its preparation method and application.
Background technology
Gold, silver have excellent optical property, these character come from the surface plasma body resonant vibration character of its uniqueness, they are widely used in multiple field, and such as surface plasma strengthens Raman, surface plasma body resonant vibration strengthens the fields such as fluorescence, photo-thermal therapy, bio-imaging, catalysis.The position at the surface plasmon absorption peak of anisotropic gold, silver nanometer sheet can be adjusted near infrared region, this is most important in the application of biological field for gold, silver, because the absorption to light of biological tissue, blood and water is minimum in this spectral region.
Scientist prepares Nano silver piece in calendar year 2001, and scientist has carried out large quantity research to the preparation of Nano silver piece and optical property after this.The preparation method of Nano silver piece has variation, high yield, the advantage such as simple and easy, and Nano silver piece has excellent optical property, these advantages make Nano silver piece demonstrate potential application prospect in some fields, but limit the extensive use of Nano silver piece due to the unstability of Nano silver piece and bio-toxicity.
In theory in the spectral region of > 600nm, the optical property of gold-nano-piece and the optical property of Nano silver piece close, be better than the optical property of gold nano grain, gold utensil has easy functionalization, good stability and biocompatibility, but gold-nano-piece does not obtain investigation and application widely, this is mainly owing to there is more problem in the preparation of gold-nano-piece, although iodide ion can improve the productive rate of gold-nano-piece, still there is the deficiencies such as productive rate is low, monodispersity is poor in gold-nano-piece.The method preparing gold-nano-piece of simple high yield becomes study hotspot.
In theory, the advantage of the advantage of silver nanoparticle crystalline substance and gold can be combined with each other by epitaxial growth method.The lattice paprmeter difference of Jin Yuyin is very little, and gold atom by the surface of epitaxial deposition in silver nanoparticle crystalline substance, can form the silver-gold nanocrystals of nucleocapsid structure.This nanocrystallinely have multiple character and advantage, the stability of such as gold, easily functionalization, good biocompatibility and optical property, the diversity of silver and excellent optical property etc.Because the oxidation-reduction potential of gold chloride is higher than the oxidation-reduction potential of silver, the spontaneous generation displacement reaction of meeting between gold chloride and silver nanoparticle crystalline substance, the structures such as the nanocages of formation electrum or nanometer framework, and the stability of these structures existing problems.Scientist attempts, by regulating thermodynamics of reactions and dynamics to suppress displacement reaction, to make gold atom be deposited on the surface of silver nanoparticle crystalline substance by epitaxially grown method, thus obtain the silver-gold nanocrystals of nucleocapsid structure.Dynamics regulates and mainly comprises the pH value regulating reaction system and the speed etc. of adding golden presoma; Thermodynamics regulates the oxidation-reduction potential then mainly by selecting suitable part to reduce gold.Such as, but these methods still Shortcomings, manufacturing cycle is long, process is complicated, there is the problems such as displacement reaction.
Summary of the invention
The object of the present invention is to provide a kind of silver-gold-nano-piece based on epitaxially grown nucleocapsid structure and its preparation method and application, the method can make gold atom in Nano silver piece surface epitaxial growth, obtained nucleocapsid structure silver-gold-nano-piece has excellent stability and optical property, has a good application prospect in organic molecule context of detection.
For achieving the above object, the technical solution used in the present invention is:
Based on a preparation method for the silver-gold-nano-piece of epitaxially grown nucleocapsid structure, comprise the following steps:
1) Nano silver piece solution is prepared
Silver nitrate is added to the water, is mixed with liquor argenti nitratis ophthalmicus, then add trisodium citrate, hydrogen peroxide and sodium borohydride aqueous solution successively wherein, stir 0.2 ~ 6h, obtain Nano silver piece solution; Wherein the mol ratio of silver nitrate, trisodium citrate, hydrogen peroxide, sodium borohydride is 1:(5 ~ 100): (50 ~ 1000): (1 ~ 50);
2) precursor solution of preparation gold
Gold chloride, part and pH adjusting agent are added to the water, obtain the mixed liquor that pH value is 8 ~ 12, mixed liquor is left standstill 0.5 ~ 72h at 4 ~ 80 DEG C, obtain the precursor solution of gold; Wherein the mol ratio of gold chloride and part is 1:(3 ~ 15);
3) nucleocapsid structure silver-gold-nano-piece is prepared
Water is added in the precursor solution of gold, be mixed with the precursor water solution of gold, then surfactant and reducing agent is added wherein, and add acetonitrile or part, make the gold element in the precursor water solution of gold, reducing agent, surfactant, the mol ratio of acetonitrile is 1:(1 ~ 100): (1 ~ 1000): (100 ~ 20000), or make the gold element in the precursor water solution of gold, reducing agent, surfactant, the mol ratio of part is 1:(1 ~ 100): (1 ~ 1000): (1 ~ 100), then add pH adjusting agent and pH value is adjusted to 8 ~ 12, add Nano silver piece solution again, obtain mixture, in mixture, the mol ratio of gold element and silver element is 1:(1 ~ 6), mixture is left standstill reaction 0.5 ~ 72h at 4 ~ 80 DEG C, after reaction terminates, product is centrifugal, washing, namely silver-the gold-nano-piece of nucleocapsid structure is obtained.
Described step 1) in the concentration of liquor argenti nitratis ophthalmicus be 1 × 10
-5~ 1 × 10
-3mol/L;
Described step 2) in mixed liquor the concentration of gold chloride be 1 × 10
-5~ 2 × 10
-1mol/L;
Described step 3) in the concentration of precursor water solution of gold be 1 × 10
-6~ 1 × 10
-2mol/L.
In step 2) carry out before first to step 1) size of Nano silver piece in obtained Nano silver piece solution regulates, concrete regulating step is: get the step 1 that volume is V1) obtained Nano silver piece solution, be scattered in after it is centrifugal in water, obtain the Nano silver piece dispersion liquid that volume is V2, V1:V2=1:(0.5 ~ 10), in Nano silver piece dispersion liquid, add trisodium citrate and ascorbic acid, obtain solution A, in solution A, the molar concentration of ascorbic acid is 1 × 10
-5~ 1 × 10
-1mol/L, the molar concentration of trisodium citrate is 1 × 10
-5~ 1 × 10
-2mol/L; The mixed aqueous solution of preparation natrium citricum and silver nitrate, be designated as B solution, in B solution, the concentration of silver nitrate is 1 × 10
-5~ 1 × 10
-2mol/L, the molar concentration of trisodium citrate is 1 × 10
-5~ 1 × 10
-2mol/L; B solution is dropwise joined in solution A, at room temperature reacts, when the UV, visible light near ir absorption peaks measuring reaction system be greater than 600nm be less than or equal to 3000nm time, stop drip B solution, obtain the Nano silver piece solution of different size.
The average-size of the Nano silver piece in the Nano silver piece solution after adjustment is 30nm ~ 5 μm.
Described part is sulphite, bisulfites or thiosulfate.
Described pH adjusting agent is NaOH, potassium hydroxide, sodium carbonate, potash, sodium acid carbonate, saleratus, sodium hydrogen phosphate, dipotassium hydrogen phosphate or ammoniacal liquor.
Described surfactant is polyvinylpyrrolidone, polyoxyethylene-poly-oxypropylene polyoxyethylene triblock copolymer, dodecyl sodium sulfate or softex kw.
Described reducing agent is ascorbic acid, hydroxylamine hydrochloride, formaldehyde, hydrazine hydrate or boron hydride.
Silver-the gold-nano-piece of the nucleocapsid structure that the preparation method of the described silver-gold-nano-piece based on epitaxially grown nucleocapsid structure obtains, this silver-gold-nano-piece is made up of kernel portion and housing parts, wherein kernel portion is Nano silver piece, and housing parts is by gold nano layer that epitaxial growth goes out on Nano silver piece.
The application of silver-gold-nano-piece in the Raman substrate for the preparation of detection organic molecule of described nucleocapsid structure.
Compared with prior art, beneficial effect of the present invention is:
The preparation method of the silver-gold-nano-piece based on epitaxially grown nucleocapsid structure provided by the invention, first is that raw material obtains Nano silver piece solution with silver nitrate, then by gold chloride and part soluble in water, adding pH adjusting agent adjust ph is 8 ~ 12, be obtained by reacting gold precursor solution; Again reducing agent, surfactant, pH adjusting agent, part or acetonitrile, Nano silver piece solution are added in the precursor solution of gold, be obtained by reacting nucleocapsid structure Fa Yin-gold-nano-piece.In the present invention, part can form golden presoma with gold chloride root generation coordination, the oxidation-reduction potential of the presoma of the gold obtained by coordination is lower than the oxidation-reduction potential of silver, the oxidation-reduction potential of gold can be reduced, thus stoping presoma and the Nano silver piece generation displacement reaction of gold, part can not produce serious etching to silver strip simultaneously.The present invention is using Nano silver piece as seed, and utilize reducing agent that the presoma of gold is reduced to gold atom, gold atom is coated on the top layer of Nano silver piece by epitaxially grown mode, in Nano silver piece surface epitaxial growth, forms the silver-gold-nano-piece of nucleocapsid structure.Preparation process of the present invention is simple, and preparation method is easy, and the cycle is short, and productive rate is high, reproducible, is applicable to large-scale production.Pattern and the size of the silver-gold-nano-piece of obtained nucleocapsid structure are controlled, and the silver-gold-nano-piece of the nucleocapsid structure of preparation has the advantages such as excellent stability and good optical property, has broad application prospects in fields such as organic molecule detections.
Further, the present invention, after obtained Nano silver piece solution, can adjust the size of the Nano silver piece in Nano silver piece solution, thus the Nano silver piece of different size can be provided as seed; And by the silver-gold-nano-piece using the Nano silver piece of different size can prepare the nucleocapsid structure of different size as seed; And the deposition of gold atom on Nano silver piece can be regulated by controlling reaction condition; And can, by controlling different growth conditions, make the silver-gold-nano-piece of the nucleocapsid structure obtained present various structures.
Further, silver-the gold-nano-piece of the nucleocapsid structure that the present invention obtains shows good stability and optical property, silver-the gold-nano-piece of this nucleocapsid structure is placed in the corrosive atmosphere such as hydrogen peroxide, ferric trichloride measuring stability, and test result shows that the stability of the silver-gold-nano-piece of this nucleocapsid structure is consistent with the stability of gold; And the silver-gold-nano-piece of this nucleocapsid structure has excellent surface plasma body resonant vibration performance, silver-the gold-nano-piece of nucleocapsid structure is used as the detection that Raman matrix is used for organic molecule (as crystal violet), result shows: the laser that crystal violet is 532nm at solid phase wavelength carries out Raman detection, and the concentration limits of detection can reach 10
-8mol/L; Crystal violet molecule carries out Raman detection with the laser that wavelength is 633nm in water, and the detectable concentration limit in water can reach 10
-7mol/L, the silver-gold-nano-piece of nucleocapsid structure that therefore the present invention obtains is expected to be used widely, especially at biological field.
Accompanying drawing explanation
Fig. 1 is the transmission electron micrograph of the silver-gold-nano-piece of the nucleocapsid structure that the embodiment of the present invention 1 obtains.
Fig. 2 is transmission electron micrograph and the high angle annular dark field-scanning projection electron transmission micrographs sheet of the silver-gold-nano-piece of the nucleocapsid structure that the embodiment of the present invention 2 obtains, wherein (a) is transmission electron micrograph, and (b) is high angle annular dark field-scanning projection electron transmission micrographs sheet.
Fig. 3 is the transmission electron micrograph of the silver-gold-nano-piece of the nucleocapsid structure that the embodiment of the present invention 3 obtains.
Fig. 4 is the transmission electron microscope photo of the silver-gold-nano-piece of the nucleocapsid structure that the embodiment of the present invention 4 obtains.
Fig. 5 is the transmission electron microscope photo of the silver-gold-nano-piece of the nucleocapsid structure that the embodiment of the present invention 5 obtains.
Fig. 6 is the transmission electron microscope photo of the silver-gold-nano-piece of the nucleocapsid structure that the embodiment of the present invention 6 obtains.
Fig. 7 is the transmission electron microscope photo of silver-gold-nano-piece in strong oxidizing property and corrosive environment after stability test of the nucleocapsid structure that the embodiment of the present invention 1 obtains, wherein (a) is the transmission electron microscope photo after stability test in hydrogen peroxide, and (b) is the transmission electron microscope photo after stability test in ferric trichloride.
Fig. 8 is that the Raman of the silver-gold-nano-piece of the nucleocapsid structure that the embodiment of the present invention 1 obtains strengthens test, silver-gold-nano-piece that wherein (a) is nucleocapsid structure strengthens test to the Raman of crystal violet (CV) in atmosphere, and silver-gold-nano-piece that (b) is nucleocapsid structure strengthens test to the Raman of CV in water.
Detailed description of the invention
Provide several preferably embodiment of the present invention below, be further illustrate of the present invention, instead of limit the scope of the invention.
Embodiment 1:
(1) silver nitrate is added to the water, makes its molar concentration be 1 × 10
-4mol/L, adds trisodium citrate, hydrogen peroxide afterwards, then adds sodium borohydride aqueous solution fast, and the mol ratio of silver nitrate, trisodium citrate, hydrogen peroxide, sodium borohydride is 1:45:240:6, stirs 0.5h, obtains Nano silver piece solution.The UV, visible light near ir absorption peaks of this Nano silver piece solution is 600nm, and the average-size of the Nano silver piece in this Nano silver piece solution is 30nm.
(2) precursor solution of preparation gold.Gold chloride, part (sodium sulfite), pH adjusting agent (NaOH) are added to the water, make the concentration of gold chloride be 1.25 × 10
-3mol/L, the mol ratio of gold chloride and part is 1:3, and the pH value of solution is 10, at 25 DEG C, leave standstill 12h, obtains the precursor solution of gold.
(3) nucleocapsid structure silver-gold-nano-piece is prepared.The precursor concentration of configuration gold is 5 × 10
-4the aqueous solution of mol/L, add surfactant (polyvinylpyrrolidone), reducing agent (ascorbic acid), part (sodium sulfite), the mol ratio of gold element, reducing agent, surfactant, sodium sulfite is made to be 1:20:100:1, the pH value adding sodium hydrate regulator solution is 8, add in above-mentioned solution after getting Nano silver piece solution centrifugal prepared by step (1), GOLD FROM PLATING SOLUTION is made to be 1:1 with the mol ratio of silver, 12h is left standstill at 30 DEG C, centrifuge washing, obtains the silver-gold-nano-piece of nucleocapsid structure.
Fig. 1 is the transmission electron micrograph of the silver-gold-nano-piece of the nucleocapsid structure that the embodiment of the present invention 1 obtains.In Fig. 1 (a), (b), the light-colored part of nanometer sheet is silver, and dark parts is gold, and Nano silver piece is coated by golden shell.
Embodiment 2:
(1) silver nitrate is added to the water, makes its molar concentration be 1 × 10
-4mol/L, adds trisodium citrate, hydrogen peroxide afterwards, then adds sodium borohydride aqueous solution fast, and the mol ratio of silver nitrate, trisodium citrate, hydrogen peroxide, sodium borohydride is 1:80:350:18, stirs 2h, obtains Nano silver piece solution.
(2) precursor solution of preparation gold.Gold chloride, part (sodium sulfite), pH adjusting agent (NaOH) are added to the water, make the concentration of gold chloride be 5 × 10
-4mol/L, the mol ratio of gold chloride and part is 1:3, and the pH value of solution is 12, at 30 DEG C, leave standstill 8h, obtains the precursor solution of gold.
(3) nucleocapsid structure silver-gold-nano-piece is prepared.The precursor concentration of configuration gold is 5 × 10
-4the aqueous solution of mol/L, add surfactant (polyvinylpyrrolidone), reducing agent (ascorbic acid), acetonitrile, the mol ratio of golden presoma, reducing agent, surfactant, acetonitrile is made to be 1:20:100:4000, the pH value adding sodium hydrate regulator solution is 10, add in above-mentioned solution after getting Nano silver piece solution centrifugal prepared by step (1), GOLD FROM PLATING SOLUTION is made to be 1:1 with the mol ratio of silver, at 25 DEG C of standing 16h, centrifuge washing, obtains the silver-gold-nano-piece of nucleocapsid structure.
Fig. 2 is transmission electron micrograph and the high angle annular dark field-scanning projection electron transmission micrographs sheet of the silver-gold-nano-piece of the nucleocapsid structure that the embodiment of the present invention 2 obtains, wherein (a) is transmission electron micrograph, in picture, the light areas of nanometer sheet is silver, dark parts is gold, b () is high angle annular dark field-scanning projection electron transmission micrographs sheet, in picture, nanometer sheet edge bright areas is gold, and middle dull areas is silver; Nano silver piece is coated by golden shell, and overall is the structures such as hexagon.
Embodiment 3:
(1) silver nitrate is added to the water, makes its molar concentration be 1 × 10
-4mol/L, adds trisodium citrate, hydrogen peroxide afterwards, then adds sodium borohydride aqueous solution fast, and the mol ratio of silver nitrate, trisodium citrate, hydrogen peroxide, sodium borohydride is 1:60:300:10, stirs 1h, obtains Nano silver piece solution.
(2) precursor solution of preparation gold.Gold chloride, part (sodium sulfite), pH adjusting agent (potassium hydroxide) are added to the water, make the concentration of gold chloride be 5 × 10
-3mol/L, the mol ratio of gold chloride and part is 1:5, and the pH value of solution is 10, at 25 DEG C, leave standstill 8h, obtains the precursor solution of gold.
(3) nucleocapsid structure silver-gold-nano-piece is prepared.The precursor concentration of configuration gold is 1 × 10
-3the aqueous solution of mol/L, add surfactant (polyvinylpyrrolidone), reducing agent (ascorbic acid), part, the mol ratio of golden presoma, reducing agent, surfactant, part is made to be 1:10:40:1, adding potassium hydroxide regulates the pH value of solution to be 10, add in above-mentioned solution after getting Nano silver piece solution centrifugal prepared by step (1), GOLD FROM PLATING SOLUTION is made to be 1:1 with the mol ratio of silver, at 30 DEG C of standing 12h, centrifuge washing, obtains the silver-gold-nano-piece of nucleocapsid structure.
Fig. 3 is the transmission electron micrograph of the silver-gold-nano-piece of the nucleocapsid structure that the embodiment of the present invention 3 obtains, and in Fig. 3, the light-colored part of nanometer sheet is silver, and dark parts is gold, and Nano silver piece is coated by golden shell.
Embodiment 4:
(1) silver nitrate is added to the water, makes its molar concentration be 1 × 10
-4mol/L, adds trisodium citrate, hydrogen peroxide afterwards, then adds sodium borohydride aqueous solution fast, and the mol ratio of silver nitrate, trisodium citrate, hydrogen peroxide, sodium borohydride is 1:45:250:6, stirs 0.5h, obtains Nano silver piece solution.
(2) get Nano silver piece solution prepared by step (1) that volume is V1 it is centrifugal after be scattered in water, obtain the Nano silver piece dispersion liquid that volume is V2, V1:V2=1:1, in Nano silver piece dispersion liquid, add trisodium citrate and ascorbic acid, make the molar concentration of ascorbic acid be 1.5 × 10
-3mol/L, the molar concentration of trisodium citrate is 5 × 10
-4mol/L, this mixed solution is designated as solution A; The mixed aqueous solution of preparation natrium citricum and silver nitrate, makes the molar concentration of silver nitrate be 7.5 × 10
-4mol/L, the molar concentration of trisodium citrate is 5 × 10
-4mol/L, this mixed solution is designated as B solution; B solution is dropwise joined in solution A, at room temperature react, when the UV, visible light near ir absorption peaks measuring reaction system is positioned at 880nm, stop dripping B solution (stopping reaction), in the Nano silver piece solution obtained, the average-size of Nano silver piece is 175nm.
(3) precursor solution of preparation gold.Gold chloride, part (sodium sulfite), pH adjusting agent (potash) are added to the water, make the concentration of gold chloride be 5 × 10
-3mol/L, the mol ratio of gold chloride and part is 1:3, and the pH value of solution is 8, at 60 DEG C, leave standstill 4h, obtains the precursor solution of gold.
(4) nucleocapsid structure silver-gold-nano-piece is prepared.The precursor concentration of configuration gold is 5 × 10
-4the aqueous solution of mol/L, add surfactant (polyvinylpyrrolidone), reducing agent (ascorbic acid), part (sodium sulfite), the mol ratio of golden presoma, reducing agent, surfactant, part is made to be 1:16:100:4, adding potash regulates the pH value of solution to be 10, add in above-mentioned solution after getting Nano silver piece solution centrifugal prepared by step (1), GOLD FROM PLATING SOLUTION is made to be 1:2 with the mol ratio of silver, at 40 DEG C of standing 6h, centrifuge washing, obtains the silver-gold-nano-piece of nucleocapsid structure.
Fig. 4 is the transmission electron microscope photo of the silver-gold-nano-piece of the nucleocapsid structure that the embodiment of the present invention 4 obtains, and in figure, the light-colored part of nanometer sheet is silver, and dark parts is gold, and Nano silver piece is coated by golden shell, the edge indentation of outer gold.
Embodiment 5:
(1) silver nitrate is added to the water, makes its molar concentration be 1 × 10
-4mol/L, adds trisodium citrate, hydrogen peroxide afterwards, then adds sodium borohydride aqueous solution fast, and the mol ratio of silver nitrate, trisodium citrate, hydrogen peroxide, sodium borohydride is 1:45:250:6, stirs 0.5h, obtains Nano silver piece solution.
(2) get Nano silver piece solution prepared by step (1) that volume is V1 it is centrifugal after be scattered in water, obtain the Nano silver piece dispersion liquid that volume is V2, V1:V2=1:0.5, in Nano silver piece dispersion liquid, add trisodium citrate and ascorbic acid, make the molar concentration of ascorbic acid be 4 × 10
-4mol/L, the molar concentration of trisodium citrate is 1 × 10
-3mol/L, this mixed solution is designated as solution A; The mixed aqueous solution of preparation natrium citricum and silver nitrate, makes the molar concentration of silver nitrate be 4 × 10
-4mol/L, the molar concentration of trisodium citrate is 2 × 10
-4mol/L, this mixed solution is designated as B solution; B solution is dropwise joined in solution A, at room temperature react, when the UV, visible light near ir absorption peaks measuring reaction system is positioned at 780nm, stop dripping B solution (stopping reaction), in the Nano silver piece solution obtained, the average-size of Nano silver piece is 132nm.
(3) precursor solution of preparation gold.Gold chloride, part (sodium sulfite), pH adjusting agent (sodium acid carbonate) are added to the water, make the concentration of gold chloride be 1 × 10
-3mol/L, the mol ratio of gold chloride and part is 1:5, and the pH value of solution is 10, at 40 DEG C, leave standstill 8h, obtains the precursor solution of gold.
(4) nucleocapsid structure silver-gold-nano-piece is prepared.The precursor concentration of configuration gold is 5 × 10
-4the aqueous solution of mol/L, add surfactant (polyvinylpyrrolidone), reducing agent (ascorbic acid), part (sodium sulfite), the mol ratio of golden presoma, reducing agent, surfactant, part is made to be 1:12:40:6, the pH value adding manganese hydrogen sodium regulating solution is 10, add in above-mentioned solution after getting Nano silver piece solution centrifugal prepared by step (1), GOLD FROM PLATING SOLUTION is made to be 1:4 with the mol ratio of silver, at 40 DEG C of standing 6h, centrifuge washing, obtains the silver-gold-nano-piece of nucleocapsid structure.
Fig. 5 is the transmission electron microscope photo of the silver-gold-nano-piece of the nucleocapsid structure that the embodiment of the present invention 5 obtains, and in figure, the light-colored part of nanometer sheet is silver, and dark parts is gold, and Nano silver piece is coated by golden shell.
Embodiment 6:
(1) silver nitrate is added to the water, makes its molar concentration be 1 × 10
-4mol/L, adds trisodium citrate, hydrogen peroxide afterwards, then adds sodium borohydride aqueous solution fast, and the mol ratio of silver nitrate, trisodium citrate, hydrogen peroxide, sodium borohydride is 1:80:350:18, stirs 2h, obtains Nano silver piece solution.
(2) get Nano silver piece solution prepared by step (1) that volume is V1 it is centrifugal after be scattered in water, obtain the Nano silver piece dispersion liquid that volume is V2, V1:V2=1:0.5, in Nano silver piece dispersion liquid, add trisodium citrate and ascorbic acid, make the molar concentration of ascorbic acid be 2 × 10
-3mol/L, the molar concentration of trisodium citrate is 2 × 10
-3mol/L, this mixed solution is designated as solution A; The mixed aqueous solution of preparation natrium citricum and silver nitrate, makes the molar concentration of silver nitrate be 1 × 10
-4mol/L, the molar concentration of trisodium citrate is 1 × 10
-4mol/L, this mixed solution is designated as B solution; B solution is dropwise joined in solution A, at room temperature react, when the UV, visible light near ir absorption peaks measuring reaction system is positioned at 780nm, stop dripping B solution (stopping reaction), in the Nano silver piece solution obtained, the average-size of Nano silver piece is 218nm.
(3) precursor solution of preparation gold.Gold chloride, part (sodium sulfite), pH adjusting agent (NaOH) are added to the water, make the concentration of gold chloride be 5 × 10
-4mol/L, the mol ratio of gold chloride and part is 1:3, and the pH value of solution is 12, at temperature 80 DEG C, leave standstill 1h, obtains the precursor solution of gold.
(4) nucleocapsid structure silver-gold-nano-piece is prepared.The precursor concentration of configuration gold is 5 × 10
-4the aqueous solution of mol/L, add surfactant (polyvinylpyrrolidone), reducing agent (ascorbic acid), part (sodium sulfite), the mol ratio of golden presoma, reducing agent, surfactant, part is made to be 1:20:100:2, the pH value adding sodium hydrate regulator solution is 12, add in above-mentioned solution after getting Nano silver piece solution centrifugal prepared by step (1), GOLD FROM PLATING SOLUTION is made to be 1:6 with the mol ratio of silver, at 25 DEG C of standing 12h, centrifuge washing, obtains the silver-gold-nano-piece of nucleocapsid structure.
Fig. 6 is the transmission electron microscope photo of the silver-gold-nano-piece of the nucleocapsid structure that the embodiment of the present invention 6 obtains, and in figure, the light-colored part of nanometer sheet is silver, and dark parts is gold, and Nano silver piece is coated by golden shell.
Embodiment 7:
(1) silver nitrate is added to the water, makes its molar concentration be 5 × 10
-4mol/L, adds trisodium citrate, hydrogen peroxide afterwards, then adds sodium borohydride aqueous solution fast, and the mol ratio of silver nitrate, trisodium citrate, hydrogen peroxide, sodium borohydride is 1:25:500:30, stirs 3h, obtains Nano silver piece solution.
(2) precursor solution of preparation gold.Gold chloride, part (sodium hydrogensulfite), pH adjusting agent (dipotassium hydrogen phosphate) are added to the water, make the concentration of gold chloride be 1 × 10
-4mol/L, the mol ratio of gold chloride and part is 1:8, and the pH value of solution is 8.5, at 15 DEG C, leave standstill 50h, obtains the precursor solution of gold.
(3) nucleocapsid structure silver-gold-nano-piece is prepared.The precursor concentration of configuration gold is 1 × 10
-5the aqueous solution of mol/L, add surfactant (softex kw), reducing agent (hydrazine hydrate), acetonitrile, the mol ratio of golden presoma, reducing agent, surfactant, acetonitrile is made to be 1:1:1:100, adding dipotassium hydrogen phosphate regulates the pH value of solution to be 8.5, add in above-mentioned solution after getting Nano silver piece solution centrifugal prepared by step (1), GOLD FROM PLATING SOLUTION is made to be 1:3.5 with the mol ratio of silver, at 10 DEG C of standing 50h, centrifuge washing, obtains the silver-gold-nano-piece of nucleocapsid structure.
Embodiment 8:
(1) silver nitrate is added to the water, makes its molar concentration be 5 × 10
-3mol/L, adds trisodium citrate, hydrogen peroxide afterwards, then adds sodium borohydride aqueous solution fast, and the mol ratio of silver nitrate, trisodium citrate, hydrogen peroxide, sodium borohydride is 1:90:800:40, stirs 4h, obtains Nano silver piece solution.
(2) precursor solution of preparation gold.Gold chloride, part (potassium sulfite), pH adjusting agent (sodium carbonate) are added to the water, make the concentration of gold chloride be 1 × 10
-2mol/L, the mol ratio of gold chloride and part is 1:12, and the pH value of solution is 10.5, at 50 DEG C, leave standstill 30h, obtains the precursor solution of gold.
(3) nucleocapsid structure silver-gold-nano-piece is prepared.The precursor concentration of configuration gold is 5 × 10
-3the aqueous solution of mol/L, add surfactant (dodecyl sodium sulfate), reducing agent (sodium borohydride), acetonitrile, the mol ratio of golden presoma, reducing agent, surfactant, acetonitrile is made to be 1:100:1000:20000, the pH value adding sodium carbonate regulating solution is 10.5, add in above-mentioned solution after getting Nano silver piece solution centrifugal prepared by step (1), GOLD FROM PLATING SOLUTION is made to be 1:2.5 with the mol ratio of silver, at 60 DEG C of standing 20h, centrifuge washing, obtains the silver-gold-nano-piece of nucleocapsid structure.
Embodiment 9:
(1) silver nitrate is added to the water, makes its molar concentration be 1 × 10
-5mol/L, adds trisodium citrate, hydrogen peroxide afterwards, then adds sodium borohydride aqueous solution fast, and the mol ratio of silver nitrate, trisodium citrate, hydrogen peroxide, sodium borohydride is 1:5:50:1, stirs 0.2h, obtains Nano silver piece solution.
(2) get Nano silver piece solution prepared by step (1) that volume is V1 it is centrifugal after be scattered in water, obtain the Nano silver piece dispersion liquid that volume is V2, V1:V2=1:5, in Nano silver piece dispersion liquid, add trisodium citrate and ascorbic acid, make the molar concentration of ascorbic acid be 1 × 10
-5mol/L, the molar concentration of trisodium citrate is 1 × 10
-5mol/L, this mixed solution is designated as solution A; The mixed aqueous solution of preparation natrium citricum and silver nitrate, makes the molar concentration of silver nitrate be 1 × 10
-5mol/L, the molar concentration of trisodium citrate is 1 × 10
-5mol/L, this mixed solution is designated as B solution; B solution is dropwise joined in solution A, at room temperature react, when the UV, visible light near ir absorption peaks measuring reaction system is positioned at 1810nm, stop dripping B solution (stopping reaction), in the Nano silver piece solution obtained, the average-size of Nano silver piece is 2.1 μm.
(3) precursor solution of preparation gold.Gold chloride, part (sodium thiosulfate), pH adjusting agent (ammoniacal liquor) are added to the water, make the concentration of gold chloride be 1 × 10
-5mol/L, the mol ratio of gold chloride and part is 1:15, and the pH value of solution is 9, at temperature 4 DEG C, leave standstill 72h, obtains the precursor solution of gold.
(4) nucleocapsid structure silver-gold-nano-piece is prepared.The precursor concentration of configuration gold is 1 × 10
-6the aqueous solution of mol/L, add surfactant (polyoxyethylene-poly-oxypropylene polyoxyethylene triblock copolymer), reducing agent (hydroxylamine hydrochloride), part (sodium thiosulfate), the mol ratio of golden presoma, reducing agent, surfactant, part is made to be 1:1:1:10, adding ammoniacal liquor regulates the pH value of solution to be 9, add in above-mentioned solution after getting Nano silver piece solution centrifugal prepared by step (1), GOLD FROM PLATING SOLUTION is made to be 1:3 with the mol ratio of silver, at 4 DEG C of standing 72h, centrifuge washing, obtains the silver-gold-nano-piece of nucleocapsid structure.
Embodiment 10:
(1) silver nitrate is added to the water, makes its molar concentration be 1 × 10
-3mol/L, adds trisodium citrate, hydrogen peroxide afterwards, then adds sodium borohydride aqueous solution fast, and the mol ratio of silver nitrate, trisodium citrate, hydrogen peroxide, sodium borohydride is 1:100:1000:50, stirs 6h, obtains Nano silver piece solution.
(2) get Nano silver piece solution prepared by step (1) that volume is V1 it is centrifugal after be scattered in water, obtain the Nano silver piece dispersion liquid that volume is V2, V1:V2=1:10, in Nano silver piece dispersion liquid, add trisodium citrate and ascorbic acid, make the molar concentration of ascorbic acid be 1 × 10
-1mol/L, the molar concentration of trisodium citrate is 1 × 10
-2mol/L, this mixed solution is designated as solution A; The mixed aqueous solution of preparation natrium citricum and silver nitrate, makes the molar concentration of silver nitrate be 1 × 10
-2mol/L, the molar concentration of trisodium citrate is 1 × 10
-2mol/L, this mixed solution is designated as B solution; B solution is dropwise joined in solution A, at room temperature react, when the UV, visible light near ir absorption peaks measuring reaction system is positioned at 3000nm, stop dripping B solution (stopping reaction), in the Nano silver piece solution obtained, the average-size of Nano silver piece is 5 μm.
(3) precursor solution of preparation gold.Gold chloride, part (potassium bisulfite), pH adjusting agent (saleratus) are added to the water, make the concentration of gold chloride be 2 × 10
-1mol/L, the mol ratio of gold chloride and part is 1:10, and the pH value of solution is 8, at temperature 75 DEG C, leave standstill 0.5h, obtains the precursor solution of gold.
(4) nucleocapsid structure silver-gold-nano-piece is prepared.The precursor concentration of configuration gold is 1 × 10
-2the aqueous solution of mol/L, add surfactant (dodecyl sodium sulfate), reducing agent (formaldehyde), part (potassium bisulfite), the mol ratio of golden presoma, reducing agent, surfactant, part is made to be 1:100:1000:100, adding saleratus regulates the pH value of solution to be 8, add in above-mentioned solution after getting Nano silver piece solution centrifugal prepared by step (1), GOLD FROM PLATING SOLUTION is made to be 1:5 with the mol ratio of silver, at 80 DEG C of standing 0.5h, centrifuge washing, obtains the silver-gold-nano-piece of nucleocapsid structure.
Below the stability of the silver-gold-nano-piece of the nucleocapsid structure that the present invention obtains and the application in detection organic molecule are described in detail.
1, stability test
Stability test is carried out to obtained nucleocapsid structure silver-gold-nano-piece, nucleocapsid structure silver-gold-nano-piece is scattered in the strong oxidizing properties such as hydrogen peroxide, ferric trichloride, nitric acid and corrosive atmosphere respectively, tests its stability.
Be specially: be scattered in by the silver-gold-nano-piece of nucleocapsid structure obtained for embodiment 1 respectively in hydrogen peroxide that concentration is 1mol/L, 0.5mol/L ferric trichloride, at 20 DEG C, leave standstill 12h, centrifuge washing, shooting transmission electron microscope photo, result as shown in Figure 7.Fig. 7 is the transmission electron microscope photo of silver-gold-nano-piece in hydrogen peroxide and ferric trichloride after stability test of the nucleocapsid structure that the embodiment of the present invention 1 obtains, wherein (a) is the transmission electron microscope photo after stability test in hydrogen peroxide, and (b) is the transmission electron microscope photo after stability test in ferric trichloride.Can find out that from 7 figure the pattern of the silver-gold-nano-piece of nucleocapsid structure does not change, still keep overall pattern.Illustrate that the silver-gold-nano-piece of the nucleocapsid structure that the present invention obtains has in strong oxidizing property and corrosive environment the stability with excellence at hydrogen peroxide, ferric trichloride etc.
2, for detecting organic molecule
Silver-the gold-nano-piece of the nucleocapsid structure that the present invention obtains can be used in detecting organic molecule.
Concrete grammar organic molecule (crystal violet) being carried out to Raman detection is: be added on several silicon chip by the hanging drop of the silver-gold-nano-piece of nucleocapsid structure obtained for the embodiment of the present invention 1, at room temperature after drying, the silver-gold-nano-piece of nucleocapsid structure is made to transfer on silicon chip; To transfer to silicon chip nucleocapsid structure silver-gold-nano-piece on to drip concentration be 10
-6mol/L is to 10
-8crystal violet (CV) solution of mol/L, and each silicon chip drips a kind of crystal violet solution of concentration, then natural drying also carries out Raman sign with the Raman instrument being equipped with wavelength 514nm, and Raman detection result is as shown in Fig. 8 (a): the sensitivity of the silver-gold-nano-piece Raman detection of the nucleocapsid structure that result display embodiment 1 obtains can reach 10
-8mol/L.Or it is 10 that the silver-gold-nano-piece of nucleocapsid structure obtained for the embodiment of the present invention 1 is scattered in concentration respectively
-5mol/L is to 10
-7in the CV solution of mol/L, leave standstill 2h, carry out Raman sign with the Raman instrument being equipped with wavelength 633nm, Raman detection result is as shown in Fig. 8 (b): the sensitivity of the Raman detection of silver-gold-nano-piece in water of the nucleocapsid structure that result display embodiment 1 obtains can reach 10
-7mol/L.
Claims (10)
1., based on a preparation method for the silver-gold-nano-piece of epitaxially grown nucleocapsid structure, it is characterized in that, comprise the following steps:
1) Nano silver piece solution is prepared
Silver nitrate is added to the water, is mixed with liquor argenti nitratis ophthalmicus, then add trisodium citrate, hydrogen peroxide and sodium borohydride aqueous solution successively wherein, stir 0.2 ~ 6h, obtain Nano silver piece solution; Wherein the mol ratio of silver nitrate, trisodium citrate, hydrogen peroxide, sodium borohydride is 1:(5 ~ 100): (50 ~ 1000): (1 ~ 50);
2) precursor solution of preparation gold
Gold chloride, part and pH adjusting agent are added to the water, obtain the mixed liquor that pH value is 8 ~ 12, mixed liquor is left standstill 0.5 ~ 72h at 4 ~ 80 DEG C, obtain the precursor solution of gold; Wherein the mol ratio of gold chloride and part is 1:(3 ~ 15);
3) nucleocapsid structure silver-gold-nano-piece is prepared
Water is added in the precursor solution of gold, be mixed with the precursor water solution of gold, then surfactant and reducing agent is added wherein, and add acetonitrile or part, make the gold element in the precursor water solution of gold, reducing agent, surfactant, the mol ratio of acetonitrile is 1:(1 ~ 100): (1 ~ 1000): (100 ~ 20000), or make the gold element in the precursor water solution of gold, reducing agent, surfactant, the mol ratio of part is 1:(1 ~ 100): (1 ~ 1000): (1 ~ 100), then add pH adjusting agent and pH value is adjusted to 8 ~ 12, add Nano silver piece solution again, obtain mixture, in mixture, the mol ratio of gold element and silver element is 1:(1 ~ 6), mixture is left standstill reaction 0.5 ~ 72h at 4 ~ 80 DEG C, after reaction terminates, product is centrifugal, washing, namely silver-the gold-nano-piece of nucleocapsid structure is obtained.
2. the preparation method of the silver-gold-nano-piece based on epitaxially grown nucleocapsid structure according to claim 1, is characterized in that: described step 1) in the concentration of liquor argenti nitratis ophthalmicus be 1 × 10
-5~ 1 × 10
-3mol/L;
Described step 2) in mixed liquor the concentration of gold chloride be 1 × 10
-5~ 2 × 10
-1mol/L;
Described step 3) in the concentration of precursor water solution of gold be 1 × 10
-6~ 1 × 10
-2mol/L.
3. the preparation method of the silver-gold-nano-piece based on epitaxially grown nucleocapsid structure according to claim 1, it is characterized in that: in step 2) carry out before first to step 1) size of Nano silver piece in obtained Nano silver piece solution regulates, concrete regulating step is: get the step 1 that volume is V1) obtained Nano silver piece solution, be scattered in after it is centrifugal in water, obtain the Nano silver piece dispersion liquid that volume is V2, V1:V2=1:(0.5 ~ 10), trisodium citrate and ascorbic acid is added in Nano silver piece dispersion liquid, obtain solution A, in solution A, the molar concentration of ascorbic acid is 1 × 10
-5~ 1 × 10
-1mol/L, the molar concentration of trisodium citrate is 1 × 10
-5~ 1 × 10
-2mol/L, the mixed aqueous solution of preparation natrium citricum and silver nitrate, be designated as B solution, in B solution, the concentration of silver nitrate is 1 × 10
-5~ 1 × 10
-2mol/L, the molar concentration of trisodium citrate is 1 × 10
-5~ 1 × 10
-2mol/L, B solution is dropwise joined in solution A, at room temperature reacts, when the UV, visible light near ir absorption peaks measuring reaction system be greater than 600nm be less than or equal to 3000nm time, stop drip B solution, obtain the Nano silver piece solution of different size.
4. the preparation method of the silver-gold-nano-piece based on epitaxially grown nucleocapsid structure according to claim 3, is characterized in that: the average-size of the Nano silver piece in the Nano silver piece solution after adjustment is 30nm ~ 5 μm.
5. the preparation method of the silver-gold-nano-piece based on epitaxially grown nucleocapsid structure according to claim 1, is characterized in that: described part is sulphite, bisulfites or thiosulfate.
6. the preparation method of the silver-gold-nano-piece based on epitaxially grown nucleocapsid structure according to claim 1, is characterized in that: described pH adjusting agent is NaOH, potassium hydroxide, sodium carbonate, potash, sodium acid carbonate, saleratus, sodium hydrogen phosphate, dipotassium hydrogen phosphate or ammoniacal liquor.
7. the preparation method of the silver-gold-nano-piece based on epitaxially grown nucleocapsid structure according to claim 1, is characterized in that: described surfactant is polyvinylpyrrolidone, polyoxyethylene-poly-oxypropylene polyoxyethylene triblock copolymer, dodecyl sodium sulfate or softex kw.
8. the preparation method of the silver-gold-nano-piece based on epitaxially grown nucleocapsid structure according to claim 1, is characterized in that: described reducing agent is ascorbic acid, hydroxylamine hydrochloride, formaldehyde, hydrazine hydrate or boron hydride.
9. silver-the gold-nano-piece of the nucleocapsid structure that the preparation method of the silver-gold-nano-piece based on epitaxially grown nucleocapsid structure in claim 1-8 described in any one obtains, it is characterized in that: this silver-gold-nano-piece is made up of kernel portion and housing parts, wherein kernel portion is Nano silver piece, and housing parts is by gold nano layer that epitaxial growth goes out on Nano silver piece.
10. the application of silver-gold-nano-piece in the Raman substrate for the preparation of detection organic molecule of nucleocapsid structure according to claim 9.
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