CN104874790A - Gold nano material adopting porous tubular hollow structure and preparation method of gold nano material - Google Patents
Gold nano material adopting porous tubular hollow structure and preparation method of gold nano material Download PDFInfo
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Abstract
The invention discloses a gold nano material adopting a porous tubular hollow structure and a preparation method of the gold nano material. The gold nano material is a tubular structure with cavities inside, a plurality of holes are formed in the surface of the gold nano material, the inner diameter of each hole is 50-500 nanometers, the thickness of a tube wall of each hole is 1-50 nanometers, and the length of each hole is 1-20 micrometers; the diameter of each hole in the tube wall is 1-50 nanometers, the thickness of the hole wall is 1-50 nanometers, and the hole in the wall is a two-dimensional or three-dimensional hole. According to the method, firstly, a silver nanowire is prepared with a polyol process to serve as a template, then, a silver-gold composite core-shell nano structure is obtained through reaction and washed with ultrapure water to be dispersed in water, a product is annealed at certain temperature, and a gold-silver alloy is obtained; the alloy is placed in concentrated nitric acid to be corroded for a period of time and is separated finally, and the gold nano material which is similar to macroscopic porous gold in shape and adopts the hollow tubular structure is obtained. According to the method, the process is simple and easy to operate, the repeatability is good, the cost is low, and the obtained gold nano material can be used for the field of chemical and electrochemical catalysis, chemical sensors, biomolecular sensors, optical information storage, drug targeting carriers, photo-thermal therapy of cancer cells and the like.
Description
Technical field
The present invention relates to nano material of a kind of perforated tubular hollow structure and preparation method thereof, refer more particularly to a kind of can be used for chemistry and electrochemical catalysis, chemical sensor, bimolecular sensors, optical information storage, drug targeting carrier, the treatment of cancer cell photo-thermal etc. pore size, porosity, wall thickness is adjustable, gold nano-material of the perforated tubular hollow structure that size is controlled and preparation method thereof.
Background technology
Since last century the people such as late nineteen eighties Japanese Scientists Haruta find the gold nano grain of load on metal oxide or active carbon there is good catalytic activity since (Masataka Haruta, Tetsuhiko Kobayashi " Methodfor theproduction of ultra-fine gold particles immobilized on a metaloxide " US Patent, 4,839,327, June 13,1989), gold as catalyst by large quantity research.And gold nano-material is just receiving strong concern in material supply section educational circles, be especially widely used in biomedical sector especially as a kind of metal material with biologically inert.The people such as rice university of U.S. Halas are at monox nanometer ball superficial growth one deck gold shell 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; NanoLett., 2007,7,1929-1934) upper extensive application.U.S.'s Washington university summer children waits in south, and to be then template with silver nano-grain obtain the nanometer shelly of gold or porose cage structure (Science, 2002,298:2176-2179 of wall by displacement reaction; Nano Lett., 2003,3:1569-1572), and in biomedicine, have application (Nano Lett., 2005,5:473-477 subsequently; Nano Lett., 2007,7:1318-1322; Nano Lett., 2007,7:3798-3802).But the adjustability that the nano material of these gold existing is core-shell structure or its optical property of cage structure is not very large, and cage structure have be only discontinuous hole and porosity is not high, specific area is large not comparatively speaking.Retrieval shows, adopting by nano silver wire is that the preparation method that template also makes its alloying obtain perforated tubular hollow structure gold nano-material by corrosion again by annealing at the gold of its surface deposition different-thickness has no report.
Summary of the invention
For 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, perforated tubular hollow structure gold nano-material that size is controlled and preparation method thereof.
The technology of preparing that the present invention takes be first with optimize polyol process to prepare required nano silver wire.Then obtained nano silver wire is scattered in certain density softex kw (or lauryl sodium sulfate, or neopelex, or polyvinylpyrrolidone, or potassium citrate, or the mixture between them) in the aqueous solution, by certain density ascorbic acid (or sodium borohydride, or citric acid, or glucose, or their mixed liquor) add in this aqueous solution as reducing agent, stir under certain mixing speed, add certain density aqueous solution of chloraurate again, stir the nucleocapsid structure that namely certain hour obtains gold and silver compound again.After methyl alcohol, milli-Q water gained gold and silver complex nucleus shell structure, gained nucleocapsid structure being scattered in again in water a period of time of annealing at a certain temperature obtains electrum, be placed in red fuming nitric acid (RFNA) again and corrode a period of time, then be separated, the final gold nano-material obtaining the perforated tubular hollow structure being similar to macroporous gold pattern.
The gold nano-material of perforated tubular hollow structure of the present invention, is characterized in that: described gold nano-material is surface is the tubular structure of cavity in cellular internal, and internal diameter is 35-650 nanometer, and pipe thickness is 1-60 nanometer, and length is 1-20 micron; On wherein said tube wall, the aperture in hole is 1-45 nanometer, and hole wall is thick is 1-45 nanometer, and wall is two dimension or three-dimensional porous.
The preparation method of the gold nano-material of above-mentioned perforated tubular hollow structure, is made up of following step:
(1) nano silver wire is prepared by polyol process;
(2) taking above-mentioned nano silver wire 0.001-0.1 gram, to be scattered in concentration be in the CTAB aqueous solution of 0.001-2 mol/L, is mixed with and does in silver atoms the nano silver wire dispersion liquid that Soviet Union is 0.001-500 mM/l;
(3) the above-mentioned nano silver wire dispersion liquid 1-50 milliliter prepared is got, and to add concentration be wherein that the aqueous ascorbic acid of 0.001-1 mol/L makes reducing agent, stir, add the HAuCl4 solution that concentration is 0.001-5 mM/l again, and under 0-90 DEG C of temperature conditions stirring reaction 2-150 minute;
(4), after above-mentioned reaction stops, centrifugal 1-50 minute with ultra-pure water cleaning and under 3000-20000 rev/min, repeats 2-10 time;
(5) sediment of above-mentioned centrifugal gained is re-dispersed in 5-50 ml water again, loads autoclave and to anneal at 20-700 DEG C 5-180 minute;
(6) after annealing, in annealing liquid, add 0.5-10 milliliter red fuming nitric acid (RFNA), and react 1-20 minute, then with ultra-pure water cleaning and under 3000-20000 rev/min centrifugal 1-50 minute, repeat 1-15 time, obtain the gold nano-material of described perforated tubular hollow structure.
In the preparation method of the gold nano-material of above-mentioned perforated tubular hollow structure: the preferred ethylene glycol of step (1) described polyalcohol, its method preparing nano silver wire is: will add in there-necked flask without water glycol, oil bath is warming up to 150 ± 15 DEG C and constant temperature 1 ± 0.2 hour, then the silver nitrate ethylene glycol solution prepared and polyvinylpyrrolidone ethylene glycol solution are added dropwise in above-mentioned there-necked flask simultaneously, constant temperature 1 ± 0.2 hour again after dripping off, then centrifugation obtains nano silver wire.
In the preparation method of the gold nano-material of above-mentioned perforated tubular hollow structure: the preferred 50-500 nanometer of diameter of step (1) described nano silver wire, the preferred 1-20 micron of length, pattern is cross section is pentagonal linear structure.
In the preparation method of the gold nano-material of above-mentioned perforated tubular hollow structure: step (2) described softex kw can substitute with dodecyl sulphonic acid or neopelex or polyvinylpyrrolidone or potassium citrate.
In the preparation method of the gold nano-material of above-mentioned perforated tubular hollow structure: the described nano silver wire dispersion liquid of step (2) in silver atoms concentration for 0.1-100 mM/l.
In the preparation method of the gold nano-material of above-mentioned perforated tubular hollow structure: step (3) described ascorbic acid can with sodium borohydride or citric acid or glucose or their mixture replacing.
In the preparation method of the gold nano-material of above-mentioned perforated tubular hollow structure: step (3) described reductant concentration is 0.001-0.1 mol/L; HAuCl4 solution concentration is 0.01-10 mM/l, and reaction temperature condition is 10-80 DEG C, and the reaction time is 10-120 minute.
Further, step (3) described reductant concentration is 0.02 mol/L; HAuCl4 solution concentration is 1 mM/l, and reaction temperature condition is 20-60 DEG C, and the reaction time is 5-80 minute.
In the preparation method of the gold nano-material of above-mentioned perforated tubular hollow structure: the preferred 8000-13000 rev/min of centrifugal rotational speed described in step (4), the preferred 3-15 minute of centrifugation time, preferred 2-6 time of number of repetition.
In the preparation method of the gold nano-material of above-mentioned perforated tubular hollow structure: the preferred 300-350 DEG C of step (5) described annealing temperature, the preferred 60-150 minute of annealing time.
In the preparation method of the gold nano-material of above-mentioned perforated tubular hollow structure: the red fuming nitric acid (RFNA) consumption described in step (6) is 1-5 milliliter, reaction time is 2-10 minute, centrifugal rotational speed is 8000-13000 rev/min, and centrifugation time is 3-15 minute, and number of repetition is 2-6 time.
The present invention is compared with the caged of existing gold or the technology of preparing of core-shell structure material, have the following advantages: perforated tubular hollow structure gold nano-material prepared by (1) the method had both maintained the pattern of original nano silver wire template, defining again inner is cavity, and wall is two dimension or three-dimensional porous novel structure; (2) its specific area of perforated tubular hollow structure gold nano-material that the method is obtained is larger, and internal cavities provides possibility for it as bio-pharmaceutical carrier simultaneously; (3) this preparation method's technique is simple, easy to operate, reproducible, relative inexpensiveness; And tradition is not high enough based on the nanocage structure porosity of the gold of displacement reaction gained, optics adjustable range is narrower, and reaction temperature is higher, complicated process of preparation, poor repeatability, and cost is high.
Accompanying drawing explanation
Fig. 1 is transmission electron microscope (TEM) figure of the gold nano-material of the perforated tubular hollow structure of preparation in the embodiment of the present invention 1.
Fig. 2 is transmission electron microscope (TEM) figure of the gold nano-material of the perforated tubular hollow structure of preparation in the embodiment of the present invention 1.
Fig. 3 is transmission electron microscope (TEM) figure of the gold nano-material of the perforated tubular hollow structure of preparation in the embodiment of the present invention 1.
Fig. 4 is transmission electron microscope (TEM) figure of the gold nano-material of the perforated tubular hollow structure of preparation in the embodiment of the present invention 1.
Fig. 5 is SEM (SEM) figure of the gold nano-material of the perforated tubular hollow structure of preparation in the embodiment of the present invention 1.
Detailed description of the invention
The embodiment below provided will the invention will be further described by reference to the accompanying drawings.
Embodiment 1:
Prepared by nano silver wire: add in 50 milliliters of there-necked flasks by 10 milliliters without water glycol, oil bath is warming up to 155 DEG C and constant temperature 1 hour, then be added dropwise in above-mentioned there-necked flask by the while of the 0.1 mol/L silver nitrate ethylene glycol solution prepared and each 6 milliliters of 0.15 mol/L polyvinylpyrrolidone ethylene glycol solution with the speed of 0.45 ml/min, constant temperature 1 hour again after dripping off, then centrifugation obtains the nano silver wire that diameter is 80-110 nanometer, length 1-20 micron.
Prepared by perforated tubular hollow structure gold nano-material: be scattered in by the nano silver wire of gained in the CTAB aqueous solution of 0.1 mol/L, add 0.04 mol/L aqueous ascorbic acid again and make reducing agent, stir under 500 revs/min of mixing speeds, and then add the aqueous solution of chloraurate 2 milliliters of 1 mM/l, more namely stirring obtains gold and silver compound nanometer nuclear shell nano-structure for 25 minutes under 30 DEG C of temperature conditions.Gained gold and silver compound nanometer nuclear shell nano-structure methyl alcohol, milli-Q water (condition: under 10000 revs/min centrifugal 15 minutes, repeat 3 times), then the sediment of above-mentioned centrifugal gained is re-dispersed in 30 ml waters again, loads autoclave and anneal 70 minutes at 350 DEG C; After annealing, to be placed in 1 milliliter of red fuming nitric acid (RFNA) corrosion reaction about 15 minutes, and then with ultra-pure water cleaning (under 12000 revs/min centrifugal 20 minutes, repeat 2 times), after separation, namely to obtain the gold nano-material of hollow tubular structure.Fig. 1 is the transmission electron microscope figure of the gold nano-material of prepared hollow tubular structure, and as seen from Figure 1 because the less corrosion of nitric acid dosage is thorough not, the pore structure on tubular structure surface is not obvious.
Embodiment 2: similar with the process of embodiment 1, but when preparing the gold nano-material of perforated tubular hollow structure, the aqueous solution of chloraurate consumption of 1 mM/l is reduced to 1 milliliter, stirring reaction time decreased to 15 minute, obtains the gold and silver compound nanometer nuclear shell nano-structure that shell is thinner.After methyl alcohol, milli-Q water, to be placed in 1 milliliter of red fuming nitric acid (RFNA) corrosion reaction after about 15 minutes centrifugation obtain hole comparatively significantly perforated tubular hollow structure gold nano-material.Fig. 2 is the transmission electron microscope figure of perforated tubular hollow structure gold nano-material, and pore size distribution is clearly as seen from Figure 2, but due to gold chloride consumption less, its tube wall is thinner.
Embodiment 3: similar with the process of embodiment 1, but when preparing the gold nano-material of perforated tubular hollow structure, the consumption of the aqueous solution of chloraurate of 1 mM/l is reduced to 0.5 milliliter, and stirring reaction time shorten is within 10 minutes, obtain the relatively thinner gold and silver compound nanometer nuclear shell nano-structure of golden shell.The all larger perforated tubular hollow structure gold nano-material of porosity and aperture is obtained after centrifugation with the corrosion of 1 milliliter of red fuming nitric acid (RFNA).Fig. 3 is the transmission electron microscope figure of perforated tubular hollow structure gold nano-material, and wall is thinner and hole is larger as seen from Figure 3.
Embodiment 4: similar with the process of embodiment 1, but when preparing the gold nano-material of perforated tubular hollow structure, red fuming nitric acid (RFNA) consumption increases to 4 milliliters, and after corrosion, also centrifugation obtains the thicker porosity of wall also higher perforated tubular hollow structure gold nano-material.Fig. 4 is the transmission electron microscope figure of hollow porous tubes shape cage structure gold nano-material, and pore size distribution is more even as seen from Figure 4.
Embodiment 5: similar with the process of embodiment 1, but when preparing nano-silver thread, regulating polyvinylpyrrolidone concentration to be 0.1 mol/L, obtaining the nano wire that diameter is 220-280 nanometer, length 1-20 micron.When preparing the gold nano-material of perforated tubular hollow structure, the consumption of the aqueous solution of chloraurate of 1 mM/l increases to 4 milliliters, and the stirring reaction time is 25 minutes nano wires obtaining gold and silver complex nucleus shell structure.Anneal 120 minutes at 300 DEG C, and then corrosion to be separated the wall obtaining hollow be the gold nanotubes of porous.The scanning electron microscope diagram of Fig. 5 to be the wall of hollow be Jenner's pipe of three-dimensional porous structure.
Claims (10)
1. a gold nano-material for perforated tubular hollow structure, is characterized in that: described gold nano-material is surface is the tubular structure of cavity in cellular internal, and internal diameter is 35-650 nanometer, and pipe thickness is 1-60 nanometer, and length is 1-20 micron; On wherein said tube wall, the aperture in hole is 1-45 nanometer, and hole wall is thick is 1-45 nanometer, and wall is two dimension or three-dimensional porous.
2. the preparation method of the gold nano-material of perforated tubular hollow structure described in claim 1, is made up of following step:
(1) nano silver wire is prepared by polyol process;
(2) taking above-mentioned nano silver wire 0.001-0.1 gram, to be scattered in concentration be in the CTAB aqueous solution of 0.001-2 mol/L, the nano silver wire dispersion liquid that to be mixed with in silver atoms concentration be 0.001-500 mM/l;
(3) get the above-mentioned nano silver wire dispersion liquid 1-50 milliliter prepared, and to add concentration be wherein that the aqueous ascorbic acid of 0.001-1 mol/L makes reducing agent, stir, then add the HAuCl that concentration is 0.001-5 mM/l
4solution, and under 0-90 DEG C of temperature conditions stirring reaction 2-150 minute;
(4), after above-mentioned reaction stops, centrifugal 1-50 minute with ultra-pure water cleaning and under 3000-20000 rev/min, repeats 2-10 time;
(5) sediment of above-mentioned centrifugal gained is re-dispersed in 5-50 ml water again, loads autoclave and to anneal at 20-700 DEG C 5-180 minute;
(6) after annealing, in annealing liquid, add 0.5-10 milliliter red fuming nitric acid (RFNA), react after 1-20 minute, then with ultra-pure water cleaning and under 3000-20000 rev/min centrifugal 1-50 minute, repeat 1-15 time, obtain the gold nano-material of described perforated tubular hollow structure.
3. the preparation method of the gold nano-material of perforated tubular hollow structure as claimed in claim 2, it is characterized in that: the diameter of step (1) described nano silver wire is 50-500 nanometer, length is 1-20 micron, and pattern is cross section is pentagonal linear structure.
4. the preparation method of the gold nano-material of perforated tubular hollow structure as claimed in claim 2, is characterized in that: step (2) described softex kw can substitute with dodecyl sulphonic acid or neopelex or polyvinylpyrrolidone or potassium citrate.
5. the preparation method of the gold nano-material of perforated tubular hollow structure as claimed in claim 2, is characterized in that: the described nano silver wire dispersion liquid of step (2) in silver atoms concentration for 0.1-100 mM/l.
6. the preparation method of the gold nano-material of perforated tubular hollow structure as claimed in claim 2, is characterized in that: step (3) described ascorbic acid can substitute with sodium borohydride or citric acid or glucose.
7. the preparation method of the gold nano-material of perforated tubular hollow structure as claimed in claim 2, is characterized in that: step (3) described reductant concentration is 0.001-0.1 mol/L; HAuCl4 solution concentration is 0.01-10 mM/l, and reaction temperature condition is 10-80 DEG C, and the reaction time is 10-120 minute.
8. the preparation method of the gold nano-material of perforated tubular hollow structure as claimed in claim 2, is characterized in that: step (3) described reductant concentration is 0.02 mol/L; HAuCl4 solution concentration is 1 mM/l, and reaction temperature condition is 20-60 DEG C, and the reaction time is 5-80 minute.
9. the preparation method of the gold nano-material of perforated tubular hollow structure as claimed in claim 2, it is characterized in that: step (5) described annealing temperature is 300-350 DEG C, annealing time is 60-150 minute.
10. the preparation method of the gold nano-material of perforated tubular hollow structure as claimed in claim 2, it is characterized in that: the red fuming nitric acid (RFNA) consumption described in step (6) is 1-5 milliliter, reaction time is 2-10 minute, centrifugal rotational speed is 8000-13000 rev/min, centrifugation time is 3-15 minute, and number of repetition is 2-6 time.
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CN110571443A (en) * | 2019-09-30 | 2019-12-13 | 福州大学 | Porous alloy nanotube catalyst with adjustable structure and preparation method thereof |
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CN111408734A (en) * | 2020-04-23 | 2020-07-14 | 华中科技大学 | Small hollow gold nanorod and preparation method and application thereof |
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Application publication date: 20150902 |
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