CN101503766B - Hollow porous tubular structured gold nano material and preparation thereof - Google Patents
Hollow porous tubular structured gold nano material and preparation thereof Download PDFInfo
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- CN101503766B CN101503766B CN2009100198539A CN200910019853A CN101503766B CN 101503766 B CN101503766 B CN 101503766B CN 2009100198539 A CN2009100198539 A CN 2009100198539A CN 200910019853 A CN200910019853 A CN 200910019853A CN 101503766 B CN101503766 B CN 101503766B
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Abstract
The invention discloses a gold nanometer material with a hollow porous tubular structure, wherein the surface of the material is porous and the inside of the material has a cavity tubular structure; the inside diameter of the tubular structure is between 50 and 500 nanometers, the thickness of the tube wall is between 1 and 50 nanometers, and the length of the tube wall is between 1 and 20 micrometers; and the aperture of upper holes of the tube wall is between 1 and 50 nanometers, the thickness of the hole wall is between 1 and 50 nanometers, and the wall is two-dimensional or three-dimensional and porous. The invention is to obtain a silver nano wire through technological synthesis of polyalcohol at first and then obtain a gold-silver composite nuclear-shell nano structure, use ultra pure water to wash the gold-silver composite nuclear-shell nano structure, disperse the gold-silver composite nuclear-shell nano structure into water, perform annealing at certain temperature to obtain gold-silver alloy, erode the gold-silver alloy in concentrated nitric acid for a period of time, and perform separation to obtain the gold nanometer material with the hollow porous tubular structure in the form of similar macroscopic porous gold. The method has the advantages of simple process, convenient operation, good repeatability and relatively low cost, and the obtained gold nanometer material can be used in the fields of chemistry, electrochemical catalysis, chemical sensors, biomolecule sensors, optical information storage, medicine-targeted vectors, photothermic treatment of cancer cells, and the like.
Description
Technical field
The present invention relates to porous tubular structured nano material of a kind of hollow and preparation method thereof, it is adjustable to refer more particularly to a kind of pore size, porosity, wall thickness that can be used for chemistry and electrochemical catalysis, chemical sensor, biomolecules transmitter, optical information storage, drug targeting carrier, the treatment of cancer cells photo-thermal etc., gold nano-material that the hollow of controllable size is porous tubular structured and preparation method thereof.
Background technology
(Masatake Haruta since last century, people such as late nineteen eighties Japan scientist Haruta found to load on gold nano grain on metal oxide or the gac to have good catalytic activity, Tetsuhiko Kobayashi " Methodfor the production of ultra-fine gold particles immobilized on a metal oxide " US Patent, 4,839,327, June 13,1989), the gold as catalyzer just by big quantity research.And gold is widely used in biomedical sector especially as a kind of metallic substance with biologically inert.People such as the Halas of U.S. rice university are at monox nanometer ball surface growth one deck gold shell and find that it has special optical property (Chem.Phys.Lett., 1998,28:243-247) and at biomedical (Proc.Natl.Acad.Sci.USA, 2003,100:13549-13554; Nano Lett., 2007,7:1929-1934) go up extensive application.U.S.'s Washington university summer children south etc. then is template obtains gold by replacement(metathesis)reaction nanometer shelly or wall foraminous cage structure (Science, 2002,298:2176-2179 with the silver nano-grain; Nano Lett., 2003,3:1569-1572), and application (Nano Lett., 2005,5:473-477 are arranged on biomedicine subsequently; NanoLett., 2007,7; 1318-1322; Nano Lett., 2007,7:3798-3802).But existing these golden nano materials are the core-shell structure or the adjustability of its optical property of cage structure is not very big, and cage structure had only is that discontinuous hole and its porosity are not high, and specific surface area is big inadequately comparatively speaking.Retrieval shows, to adopt by nano silver wire be template does not appear in the newspapers its alloying in the gold of its surface deposition different thickness and annealing again by the preparation method that corrosion obtains the porous tubular structured gold nano-material of hollow.
Summary of the invention
At the deficiencies in the prior art, the object of the present invention is to provide a kind of pore size, porosity, wall thickness is adjustable, porous tubular structured gold nano-material of hollow of controllable size and preparation method thereof.
The technology of preparing that the present invention taked is at first to prepare required nano silver wire with the polyol process of optimizing.Then prepared nano silver wire is scattered in certain density hexadecyl trimethyl ammonium bromide (or sodium laurylsulfonate or Sodium dodecylbenzene sulfonate or polyvinylpyrrolidone or Tripotassium Citrate or the mixture between the them) aqueous solution, add certain density xitix (or sodium borohydride or citric acid or glucose or their mixed solution) again and make reductive agent, under certain stirring velocity, stir, add certain density aqueous solution of chloraurate again, the restir certain hour promptly obtains gold and silver compound nucleocapsid structure.Gained gold and silver compound nucleus shell structure obtains electrum with methyl alcohol, ultrapure water washing back redispersion for some time of annealing at a certain temperature in water, be placed in the concentrated nitric acid again and corrode for some time, separate the porous tubular structured gold nano-material of hollow that promptly obtains being similar to macroscopical porous gold pattern then.
The gold nano-material that hollow of the present invention is porous tubular structured is characterized in that: porous is inner to be that the tubular structure of cavity, internal diameter are 50～500 nanometers to described gold nano-material for the surface is, and thickness of pipe is 1～50 nanometer, and length is 1～20 micron; On the wherein said tube wall aperture in hole be 1～50 nanometer, hole wall thick be 1～50 nanometer, wall be the two dimension or three-dimensional porous.
The preparation method of the gold nano-material that above-mentioned hollow is porous tubular structured, be made up of following step:
(1) prepares nano silver wire by polyol process;
(2) take by weighing above-mentioned nano silver wire 0.001～0.1 gram and be scattered in the hexadecyl trimethyl ammonium bromide aqueous solution that concentration is 0.001～2 mol, be mixed with in silver atoms concentration be 0.001～500 mmole/liter the nano silver wire dispersion liquid;
(3) get 1～50 milliliter of the above-mentioned nano silver wire dispersion liquid for preparing, and be that the aqueous ascorbic acid of 0.001～1 mol is made reductive agent, stir to wherein adding concentration, add concentration again and be 0.001～50 mmole/liter HAuCl
4Solution, and under 0～80 ℃ of temperature condition stirring reaction 5～120 minutes;
(4) after above-mentioned reaction stops, descending centrifugal 1～30 minute, repeat 2～10 times with the ultrapure water cleaning and at 5000～15000 rev/mins;
(5) throw out with above-mentioned centrifugal gained is distributed in 5～50 ml waters more again, and the autoclave of packing into was annealed 5～180 minutes down at 40～500 ℃;
(6) after the annealing, in annealing liquid, add 0.5～10 milliliter of concentrated nitric acid, and reacted 1～20 minute, descended centrifugal 1～20 minute with the ultrapure water cleaning and at 5000～15000 rev/mins again, repeat 2～10 times, promptly get the porous tubular structured gold nano-material of described hollow.
Among the preparation method of the gold nano-material that above-mentioned hollow is porous tubular structured: the preferred ethylene glycol of the described polyvalent alcohol of step (1), its method for preparing nano silver wire is: will not have water glycol and add in the there-necked flask, oil bath was warming up to 160 ± 5 ℃ and constant temperature 1 ± 0.2 hour, then Silver Nitrate ethylene glycol solution and the polyvinylpyrrolidone ethylene glycol solution for preparing is added dropwise in the above-mentioned there-necked flask simultaneously, constant temperature 1 ± 0.2 hour again after dripping off, centrifugation gets nano silver wire then.
Among the preparation method of the gold nano-material that above-mentioned hollow is porous tubular structured: preferred 50～500 nanometers of diameter of the described nano silver wire of step (1), preferred 1～20 micron of length, it is pentagonal linear structure that pattern is cross section.
Among the preparation method of the gold nano-material that above-mentioned hollow is porous tubular structured: the described hexadecyl trimethyl ammonium bromide of step (2) can also be with sodium laurylsulfonate or Sodium dodecylbenzene sulfonate or polyvinylpyrrolidone or Tripotassium Citrate or the mixture replacing between them.
Among the preparation method of the gold nano-material that above-mentioned hollow is porous tubular structured: the described nano silver wire dispersion liquid of step (2) in preferred 0.1～100 mmole of silver atoms concentration/liter.
Among the preparation method of the gold nano-material that above-mentioned hollow is porous tubular structured:: the described xitix of step (3) can be with sodium borohydride or citric acid or glucose or the mixture replacing between them.
Among the preparation method of the gold nano-material that above-mentioned hollow is porous tubular structured: preferred 0.001～0.1 mol of the described reductant concentration of step (3); HAuCl
4Preferred 0.01～10 mmole of strength of solution/liter, 10～60 ℃ of temperature of reaction condition optimizations, preferred 10～100 minutes of reaction times.
Further, preferred 0.02 mol of the described reductant concentration of step (3); HAuCl
4Preferred 1 mmole of strength of solution/liter, 20～40 ℃ of temperature of reaction condition optimizations, preferred 20～60 minutes of reaction times.
Among the preparation method of the gold nano-material that above-mentioned hollow is porous tubular structured, preferred 8000～13000 rev/mins of the described centrifugal rotational speed of step (4), preferred 3～15 minutes of centrifugation time, preferred 3～5 times of multiplicity.
Among the preparation method of the gold nano-material that above-mentioned hollow is porous tubular structured: preferred 300～350 ℃ of the described annealing temperature of step (5), preferred 60～150 minutes of annealing time.
Among the preparation method of the gold nano-material that above-mentioned hollow is porous tubular structured: the described concentrated nitric acid consumption of step (6) is preferably 1～5 milliliter, preferred 2～10 minutes of reaction times, preferred 8000～13000 rev/mins of centrifugal rotational speed, preferred 3～15 minutes of centrifugation time, preferred 3～5 times of multiplicity.
The present invention compares with the cage shape of existing gold or the technology of preparing of core-shell structure material, have the following advantages: the porous tubular structured gold nano-material of hollow of (1) this method preparation had both kept the pattern of original nano silver wire template, formed the inner cavity that is again, wall is two dimension or three-dimensional porous novel structure; (2) its specific surface area of the porous tubular structured gold nano-material of hollow of making of this method is bigger, and internal cavities is provided convenience as the bio-pharmaceutical carrier for it simultaneously; (3) this preparation method's technology is simple, easy to operate, and good reproducibility, cost are cheap relatively; And tradition is not high enough based on the nanocages shape structure porosity of the gold of replacement(metathesis)reaction gained, and the optical adjustment scope is narrower, and temperature of reaction is higher, complicated process of preparation, poor repeatability, cost height.
Description of drawings
Fig. 1 is transmission electron microscope (TEM) figure of the porous tubular structured gold nano-material of the hollow of preparation in the embodiment of the invention 1.
Fig. 2 is transmission electron microscope (TEM) figure of the porous tubular structured gold nano-material of the hollow of preparation in the embodiment of the invention 1.
Fig. 3 is transmission electron microscope (TEM) figure of the porous tubular structured gold nano-material of the hollow of preparation in the embodiment of the invention 1.
Fig. 4 is transmission electron microscope (TEM) figure of the porous tubular structured gold nano-material of the hollow of preparation in the embodiment of the invention 1.
Fig. 5 is scanning electronic microscope (SEM) figure of the porous tubular structured gold nano-material of the hollow of preparation in the embodiment of the invention 1.
Embodiment
The embodiment that below provides will the invention will be further described in conjunction with the accompanying drawings.
Embodiment 1:
Nano silver wire preparation: 10 milliliters of no water glycols are added in 50 milliliters of there-necked flasks, oil bath was warming up to 160 ℃ and constant temperature 1 hour, the speed of each 6 milliliters of while of 0.1 mol Silver Nitrate ethylene glycol solution that will prepare then and 0.15 mol polyvinylpyrrolidone ethylene glycol solution with 0.45 ml/min is added dropwise in the above-mentioned there-necked flask, constant temperature 1 hour again after dripping off, centrifugation gets the nano silver wire that diameter is 1～20 micron of 70～100 nanometer, length then.
The porous tubular structured gold nano-material preparation of hollow: prepared nano silver wire is scattered in the hexadecyl trimethyl ammonium bromide aqueous solution of 0.1 mol, add 0.04 mol aqueous ascorbic acid again and make reductive agent, under 400 rev/mins of stirring velocitys, stir, and then add 1 mmole/liter 2 milliliters of aqueous solution of chloraurate, under 40 ℃ of temperature condition, stir again and promptly obtained the compound nucleocapsid nanostructure of gold and silver in 20 minutes.The compound nucleocapsid nanostructure usefulness of gained gold and silver methyl alcohol, ultrapure water washing (condition: descended centrifugal 10 minutes at 10000 rev/mins, repeat 3 times), throw out with above-mentioned centrifugal gained is distributed in 30 ml waters more again then, and the autoclave of packing into was annealed 80 minutes down at 350 ℃; After the annealing, be placed in 1 milliliter of concentrated nitric acid corrosion reaction about 15 minutes, and then clean (12000 rev/mins centrifugal 15 minutes down, repeat 2 times), promptly obtain the gold nano-material of hollow tubular structure after the separation with ultrapure water.Fig. 1 is the transmission electron microscope figure of the gold nano-material of prepared hollow tubular structure, because the less corrosion of nitric acid dosage is thorough inadequately, the pore structure on tubular structure surface is not obvious as seen from Figure 1.
Embodiment 2: similar with the process of embodiment 1, but when the porous tubular structured gold nano-material of preparation hollow, 1 mmole/liter the aqueous solution of chloraurate consumption be reduced to 1 milliliter, stirring reaction time decreased to 10 minute obtains the thin compound nucleocapsid nanostructure of gold and silver of shell.After the washing of methyl alcohol, ultrapure water, be placed on that corrosion reaction corrosion back centrifugation in about 15 minutes obtains the comparatively significantly porous tubular structured gold nano-material of hollow of hole in 1 milliliter of concentrated nitric acid.Fig. 2 is the transmission electron microscope figure of the porous tubular structured gold nano-material of hollow, as seen from Figure 2 pore distribution clearly, but since the hydrochloro-auric acid consumption less, its tube wall is thinner.
Embodiment 3: similar with the process of embodiment 1, but when the porous tubular structured gold nano-material of preparation hollow, the concentrated nitric acid consumption increases to 3 milliliters, and corrosion back and centrifugation obtain the porous tubular structured gold nano-material of the also higher hollow of the thicker porosity of wall.Fig. 3 is the transmission electron microscope figure of hollow perforated tubular cage structure gold nano-material, and pore distribution is more even as seen from Figure 3.
Embodiment 4: similar with the process of embodiment 1, but when the porous tubular structured gold nano-material of preparation hollow, 1 mmole/liter the consumption of aqueous solution of chloraurate be reduced to 0.5 milliliter, the stirring reaction time shortens to 5 minutes and obtains the golden shell thinner compound nucleocapsid nanostructure of gold and silver relatively.With getting all bigger porous tubular structured gold nano-material of hollow of porosity and aperture after 1 milliliter of concentrated nitric acid corrosion and the centrifugation.Fig. 4 is the transmission electron microscope figure of the porous tubular structured gold nano-material of hollow, and wall is thin and the hole is bigger as seen from Figure 4.
Embodiment 5: similar with the process of embodiment 1, but when the preparation nano silver wire, regulating polyvinylpyrrolidone concentration is 0.1 mol, getting diameter is 250～300 nanometers, the nano wire that length is 1～20 micron.When the porous tubular structured gold nano-material of preparation hollow, 1 mmole/liter the consumption of aqueous solution of chloraurate increase to 4 milliliters, the stirring reaction time is to obtain the nano wire of gold and silver compound nucleus shell structure in 20 minutes.300 ℃ of down annealing 120 minutes, and then corrosion to separate the wall that obtains hollow be the porous gold nanotubes.Fig. 5 is the scanning electron microscope diagram of Jenner's pipe of three-dimensional porous structure for the wall of hollow.
Claims (10)
1. gold nano-material that hollow is porous tubular structured is characterized in that: porous is inner to be that the tubular structure of cavity, internal diameter are 50～500 nanometers to described gold nano-material for the surface is, and thickness of pipe is 1～50 nanometer, and length is 1～20 micron; On the wherein said tube wall aperture in hole be 1～50 nanometer, hole wall thick be 1～50 nanometer, wall be the two dimension or three-dimensional porous.
2. the preparation method of the porous tubular structured gold nano-material of the described hollow of claim 1, be made up of following step:
(1) prepares nano silver wire by polyol process;
(2) take by weighing above-mentioned nano silver wire 0.001～0.1 gram and be scattered in the hexadecyl trimethyl ammonium bromide aqueous solution that concentration is 0.001～2 mol, be mixed with in silver atoms concentration be 0.001～500 mmole/liter the nano silver wire dispersion liquid;
(3) get 1～50 milliliter of the above-mentioned nano silver wire dispersion liquid for preparing, and be that the aqueous ascorbic acid of 0.001～1 mol is made reductive agent, stir to wherein adding concentration, add concentration again and be 0.001～50 mmole/liter HAuCl
4Solution, and under 0～80 ℃ of temperature condition stirring reaction 5～120 minutes;
(4) after above-mentioned reaction stops, descending centrifugal 1～30 minute, repeat 2～10 times with the ultrapure water cleaning and at 5000～15000 rev/mins;
(5) throw out with above-mentioned centrifugal gained is distributed in 5～50 ml waters more again, and the autoclave of packing into was annealed 5～180 minutes down at 40～500 ℃;
(6) after the annealing, in annealing liquid, add 0.5～10 milliliter of concentrated nitric acid, and reacted 1～20 minute, descended centrifugal 1～20 minute with the ultrapure water cleaning and at 5000～15000 rev/mins again, repeat 2～10 times, promptly get the porous tubular structured gold nano-material of described hollow.
3. as the preparation method of the porous tubular structured gold nano-material of hollow as described in the claim 2, it is characterized in that: the diameter of the described nano silver wire of step (1) is 50～500 nanometers, and length is 1～20 micron, and it is pentagonal linear structure that pattern is cross section.
4. as the preparation method of the porous tubular structured gold nano-material of hollow as described in the claim 2, it is characterized in that: the described hexadecyl trimethyl ammonium bromide of step (2) can substitute with sodium laurylsulfonate or Sodium dodecylbenzene sulfonate or polyvinylpyrrolidone or Tripotassium Citrate.
5. as the preparation method of the porous tubular structured gold nano-material of hollow as described in the claim 2, it is characterized in that: the described nano silver wire dispersion liquid of step (2) in silver atoms concentration be 0.1～100 mmole/liter.
6. as the preparation method of the porous tubular structured gold nano-material of hollow as described in the claim 2, it is characterized in that: the described xitix of step (3) can substitute with sodium borohydride or citric acid or glucose.
7. as the preparation method of the porous tubular structured gold nano-material of hollow as described in the claim 2, it is characterized in that: the described reductant concentration of step (3) is 0.001～0.1 mol; HAuCl
4Strength of solution be 0.01～10 mmole/liter, the temperature of reaction condition is 10～60 ℃, the reaction times is 10～100 minutes.
8. as the preparation method of the porous tubular structured gold nano-material of hollow as described in the claim 7, it is characterized in that: the described reductant concentration of step (3) is 0.02 mol; HAuCl
4Strength of solution be 1 mmole/liter, the temperature of reaction condition is 20～40 ℃, the reaction times is 20～60 minutes.
9. as the preparation method of the porous tubular structured gold nano-material of hollow as described in the claim 2, it is characterized in that: the described annealing temperature of step (5) is 300～350 ℃, and annealing time is 60～150 minutes.
10. as the preparation method of the porous tubular structured gold nano-material of hollow as described in the claim 2, it is characterized in that: the described concentrated nitric acid consumption of step (6) is 1～5 milliliter, reaction times is 2～10 minutes, centrifugal rotational speed is 8000～13000 rev/mins, centrifugation time is 3～15 minutes, and multiplicity is 3～5 times.
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| CN103990793A (en) * | 2014-05-09 | 2014-08-20 | 北京威士恩科技有限公司 | High-length-to-diameter-ratio solid-walled hollow gold/gold-silver nanotube and manufacturing method thereof |
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