CN110227815A - A kind of preparation method of water dispersible nanowires of gold - Google Patents
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Abstract
The invention discloses a kind of nanowires of gold preparation methods of water dispersible, belong to technical field of nano material, first with oleyl amine as stabilizer and one-dimensional growth template, tri isopropyl silane is as efficient golden reducing agent, prepare the surface-functionalized oil-soluble nanowires of gold of oleyl amine, diameter about 2nm, draw ratio reach 1000 or more；Then with there is the oleyl amine for replacing surface hydrophobic compared with 3- mercaptopropionic acid or the thioacetic acid reagent containing thiol molecule of strong affinity with gold atom, pattern is finally prepared and keeps good, water dispersible nanowires of gold.A kind of preparation method of water dispersible nanowires of gold of the invention, the nano wire of water dispersible is obtained with hydrophilic radical method of substitution；Meanwhile by SEM as a result, it was confirmed that AuNWs pattern is good, draw ratio is kept substantially；Meanwhile should preparation method is simple, it is not only environmental-friendly but also at low cost.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of preparation method of water dispersible nanowires of gold.
Background technique
Gold nano-material such as nano particle, nanometer rods, nano-cluster are most promising nanometer materials in biomedical applications
One of material.The advantages that because of its high conductivity, easily prepared and modification, diversified nanostructure and the smallest cell toxicity, is extensive
Applied to the fields such as organizational project and medical treatment transducer part.
One-dimensional nanowires of gold (AuNWs) is great because its high aspect ratio, unique electricity, optics and magnetism cause people
Interest.Since AuNWs has biggish anisotropy and good assemble ability, nanoelectronic and molecular device are become
The important component of connection.The preparation method of AuNWs is based primarily upon template auxiliary at present, nano particle assembles, in surfactant
Jie and physical deposition etc..However, the AuNWs that these methods obtain be it is polymorphous, form is poor, and diameter is relatively large (straight
Diameter 45nm or so).Recently, the seminars such as Ravishankar report using oleyl amine or a variety of chemical substances as one-dimensional growth
The method of template and reducing agent synthesis ultra thin single crystalline AuNWs (diameter about 2nm).
From during reporting several years so far for the first time, there is researcher using long chain-amine derivative as layer growth
Template substitution oleyl amine prepares the nanowires of gold of water dispersible, but since its growth templates molecule synthesis is complicated, environment is unfriendly, consumption
When it is longer, thus be not a kind of ideal method.In addition to this there are no document reports to utilize hydrophilic radical such as sulfydryl third
Acid replaces the method for hydrophobicity oleyl amine to prepare the AuNWs of ultra-thin water dispersible.
In practical study and application, for one-dimensional nanowires of gold since the overwhelming majority is using the preparation of oleyl amine template, oil is molten
Property limits its application in water phase.Most researchs and commercially available ultra-thin AuNWs are only soluble in organic solvent at present, thus
Limit its application in the fields such as organizational project.
Compared to nanowires of gold, the gold nano-material of other structures such as gold nano grain (AuNPs), gold nanorods
(AuNRs), gold nanoclusters (AuNCs) etc., it is simple due to preparing, it is water-soluble the advantages that, in biomedical engineering field
It is with a wide range of applications by many experiments confirmation.In contrast, AuNWs has bigger draw ratio, in practical applications
May be such as compound with hydrophily functional molecular with greater advantage, especially with large biological molecule such as protein, polypeptide or
Organic copolymer it is compound etc..Therefore it is necessary for preparing the ultra-thin AuNWs of water dispersible, and requires to have both simple easy
The features such as capable, environmental-friendly, cheap.
To sum up, the AuNWs for preparing water dispersible is the primary study side of the technical field and biomedical engineering field
To having broad application prospects and researching value.
Summary of the invention
Goal of the invention: of the existing technology in order to solve the problems, such as, the present invention provides a kind of water dispersible nanowires of gold
The nanowires of gold of preparation method, preparation can be preferably scattered in aqueous phase solution.
Technical solution: in order to achieve the above-mentioned object of the invention, the present invention adopts the following technical scheme:
A kind of preparation method of water dispersible nanowires of gold, includes the following steps:
1) oil-soluble nanowires of gold is prepared
Golden precursor solution is reacted in growth templates molecule, is stood, and solution colour becomes peony from initial yellow, obtains
To nanowires of gold suspension；Then nanowires of gold suspension is purified to obtain oil-soluble nanowires of gold；
2) exchange surface hydrophilic ligand
It is handed under strong alkaline condition with the surface hydrophobic oleyl amine functional group of compounds containing thiol groups and oil-soluble nanowires of gold
Reaction is changed, finally obtains water dispersible nanowires of gold after purification.
Further, in step 1), the golden precursor solution is HAuCl4Aqueous solution, the growth templates molecule
For oleyl amine and n-hexane；By HAuCl4·3H2O is dissolved in the mixed solution of oleyl amine and n-hexane to completely rear filtering removal not
Molten object；Then tri isopropyl silane mixing is added to stand.
Further, the HAuCl4·3H2O, oleyl amine, n-hexane reaction molar concentration ratio be 10:(0.2~
0.3): (25~50).
Further, the HAuCl4The concentration of solution is 10mmol/L, and the concentration of the tri isopropyl silane is
1mmol/L。
Further, in step 1), the purifying are as follows: the anhydrous of 2~3 times of volumes is added into nanowires of gold suspension
Ethyl alcohol, piping and druming mixing, centrifugation are scattered in hexane again after removing supernatant；It repeats purification step 2~3 times.
Further, in step 2), the compounds containing thiol groups are 3- mercaptopropionic acid or thioacetic acid；Weigh 3- sulfydryl
Propionic acid or thioacetic acid are dissolved in the aqueous solution of methanol or ethyl alcohol, and adjusting pH is 12, are then added into above-mentioned be prepared into
Deionized water is added into oil-soluble nanowires of gold solution, after magnetic agitation to continue to stir.
Further, in step 2), the purifying are as follows: water intaking phase is added acetone soln centrifugation, removes acetone/3- mercapto
Base propionic acid or thioacetic acid and other impurities disperse sediment in ultrapure water again.
Further, in step 2), the purifying are as follows: water intaking phase is added to hypervelocity concentration centrifuge tube centrifugation, removes 3-
Mercaptopropionic acid or thioacetic acid and other impurities disperse sediment in ultrapure water again.
Further, the 3- mercaptopropionic acid or thioacetic acid and the molar ratio of oil-soluble nanowires of gold solution be (1~
4):1；The methanol or ethyl alcohol and water volume ratio is 10:(3~6).The concentration of the oil-soluble nanowires of gold solution is
11mg/mL。
Further, in the step 1), the time of repose is 24~48h, and reaction temperature is 25 DEG C；The step
2) in, reaction temperature is 25~37 DEG C.
The utility model has the advantages that compared with prior art, a kind of preparation method of water dispersible nanowires of gold of the invention, use is hydrophilic
Group method of substitution obtains the nano wire of water dispersible；Meanwhile by SEM as a result, it was confirmed that AuNWs pattern is good, draw ratio base
This holding；Meanwhile the preparation method have the characteristics that it is simple and easy, environmental-friendly, cheap.
Detailed description of the invention
Fig. 1 is the TEM figure for the oil-soluble AuNWs being prepared；
Fig. 2 is the SEM figure for the oil-soluble AuNWs being prepared；
Fig. 3 is the SEM figure for the water dispersible AuNWs being prepared.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples.Experimental method used in following embodiments is such as
It is conventional method without specified otherwise；Material, reagent used etc., are commercially available unless otherwise specified.
A kind of preparation method of water dispersible nanowires of gold, includes the following steps:
1) be first oil-soluble nanowires of gold preparation: golden precursor solution (HAuCl4) in growth templates molecule oleyl amine
Under help, tri isopropyl silane gradually restores Au+For gold atom, after 24~48h, solution at room temperature color by initial
Yellow becomes peony, illustrates Au+Amine compound is reduced to the nanowires of gold of oleyl amine surface modification completely, and is scattered in hexane
In solution；Then it is purified in ethyl alcohol.
2) followed by the exchange of surface hydrophilicity ligand: with the 3- having with gold atom compared with strong affinity under strong alkaline condition
Mercaptopropionic acid is exchanged with the oleyl amine of surface hydrophobic, is finally obtained pattern after purification and is kept good, water dispersible nanowires of gold.
In step 1), oil-soluble nanowires of gold specific the preparation method comprises the following steps:
Weigh the 10mmol/LHAuCl of certain mass4·3H2O, be dissolved in 0.2~0.3mmol/L oleyl amine and 25~
To complete in the mixed solution of 50mmol/L hexane, with 0.22 μm of filter filtering removal insoluble matter；1mmol/L triisopropyl is added
Silane is sufficiently mixed, and is stored at room temperature 24~48h.HAuCl4·3H2O, oleyl amine, n-hexane reaction molar concentration ratio be 10:
(0.2~0.3): (25~50).HAuCl4The concentration of solution is 10mmol/L, and the concentration of tri isopropyl silane is 1mmol/L.
In step 1), the specific purification process of oil-soluble nanowires of gold are as follows:
In nanowires of gold suspension, the dehydrated alcohol of its 2~3 times of volumes is added, sufficiently piping and druming mixing, centrifugation is gone
Clearly, it is scattered in hexane again.It repeats purification step 2~3 times.
Its oil-soluble AuNWs diameter prepared is 1.5~2nm it can be seen from Fig. 1 TEM characterization, and length is greater than 1 μm,
Surface slightly gold nano grain adheres to.
In step 2), water dispersible nanowires of gold specific the preparation method comprises the following steps:
The 3- mercaptopropionic acid or thioacetic acid for weighing 0.1~0.4mmol, are dissolved in 1~2.5mL methanol aqueous solution, adjust
Saving pH is 12, is then added into 5mL above-mentioned steps 1) it is prepared in nanowires of gold solution, magnetic agitation 30min；It is added
10~20mL deionized water continues 20~30min of stirring；Reject lower layer organic phase is added acetone soln centrifugation or is concentrated by ultrafiltration
Centrifugation is dispersed sediment in ultrapure water with removing extra acetone/3- mercaptopropionic acid or thioacetic acid and other impurities again.
It can be seen from the SEM characterization of Fig. 2-3 compared with oil-soluble AuNWs, the water dispersible AuNWs prepared exists
It in size and length, is held essentially constant, pattern becomes bended, therefore maintains physical characteristic (electricity, light, the magnetic of ultra-thin AuNWs
Etc. properties).
Step 1) reaction temperature is 25 DEG C.Step 2) reaction temperature is 25~37 DEG C.
Main raw material(s) used in following embodiment:
Three hydration gold chloride (HAuCl4·3H2O), it is purchased from Sinopharm Chemical Reagent Co., Ltd.；
Oleyl amine, tri isopropyl silane, 3- thioacetic acid (3- mercaptopropionic acid), have purchased from Shanghai Aladdin biochemical technology share
Limit company.
The preparation and purification of 1 oil-soluble AuNWs of embodiment
A) 20mg HAuCl is weighed4·3H2O is dissolved in the 5mL seed bottle of oleyl amine containing 6mL and 26mL hexane, is sufficiently shaken
Dissolution is swung, then with 0.22 μm of filter filtering removal insoluble matter；
B) 8mL tri isopropyl silane solution, oscillation mixing is added；
C) seed bottle is placed in 25 DEG C of water-baths, stands reaction for 24 hours, obtains crude product；
D) 5mL dehydrated alcohol, sufficiently piping and druming mixing is added in the AuNWs crude product solution for taking above-mentioned 2.5mL preparation, it is seen that
AuNWs Precipitation；
E) it is centrifuged 5min in 4000rpm revolving speed, removes supernatant, precipitating rejoins the dispersion of 2.5mL hexane；
In the process, it purifies 2~3 times, maximumlly reduces the presence of gold nano grain.
The preparation and purification of 2 oil-soluble AuNWs of embodiment
A) 50mg HAuCl is weighed4·3H2O is dissolved in the 100mL beaker of oleyl amine containing 1.8mL and 50mL hexane, sufficiently
Oscillation dissolution, then with 0.22 μm of filter filtering removal insoluble matter；
B) 2.5mL tri isopropyl silane solution, sealing is added, magnetic agitation is uniformly mixed；
C) beaker is placed in 25 DEG C of water-baths, stands reaction 48h, obtains crude product；
D) 7.5mL dehydrated alcohol is added in the AuNWs crude product solution for taking above-mentioned 2.5mL preparation, and sufficiently piping and druming mixing can
See AuNWs Precipitation；
E) it is centrifuged 5min in 4000rpm revolving speed, removes supernatant, precipitating rejoins the dispersion of 2.5mL hexane；
In the process, it purifies 2~3 times, maximumlly reduces the presence of gold nano grain.
The preparation and purification of 3 oil-soluble AuNWs of embodiment
A) 44mg HAuCl is weighed4·3H2O is dissolved in the 100mL beaker of oleyl amine containing 1.5mL and 40mL hexane, sufficiently
Oscillation dissolution, then with 0.22 μm of filter filtering removal insoluble matter；
B) 2.1mL tri isopropyl silane solution, sealing is added, magnetic agitation is uniformly mixed；
C) beaker is placed in 25 DEG C of water-baths, stands reaction for 24 hours, obtains crude product；
D) 5mL dehydrated alcohol, sufficiently piping and druming mixing is added in the AuNWs crude product solution for taking above-mentioned 2.5mL preparation, it is seen that
AuNWs Precipitation；
E) it is centrifuged 5min in 4000rpm revolving speed, removes supernatant, precipitating rejoins the dispersion of 2.5mL hexane；
The preparation and purification of 4 oil-soluble AuNWs of embodiment
A) 30mg HAuCl is weighed4·3H2O is dissolved in the 50mL beaker of oleyl amine containing 1mL and 20mL hexane, is sufficiently vibrated
Dissolution, then with 0.22 μm of filter filtering removal insoluble matter；
B) 1.5mL tri isopropyl silane solution, sealing is added, magnetic agitation is uniformly mixed；
C) beaker is placed in 25 DEG C of water-baths, stands reaction for 24 hours, obtains crude product；
D) 7.5mL dehydrated alcohol is added in the AuNWs crude product solution for taking above-mentioned 2.5mL preparation, and sufficiently piping and druming mixing can
See AuNWs Precipitation；
E) it is centrifuged 5min in 4000rpm revolving speed, removes supernatant, precipitating rejoins the dispersion of 2.5mL hexane；
The preparation and purification of the AuNWs of 5 water dispersible of embodiment
A) 0.123g is weighed, the 3- mercaptopropionic acid of 0.1mmol is dissolved in the solution of 1mL methanol and 0.3mL water,
Adjusting pH value of solution with 40%NaOH solution is 12；
B) measure 5mL 1) in oil-soluble AuNWs solution after purification, 1.3mLa is added) in the mercaptopropionic acid containing 3- mixing
Solution, 37 DEG C of magnetic agitation 30min；
C) 10mL deionized water is added to continue to stir 20min, AuNWs is transferred in water phase by organic phase at this time；
D) lower layer's organic phase is removed, 20mL acetone is added；4000rpm is centrifuged 5min, removes supernatant, and deionized water is added and divides again
It dissipates.
The preparation and purification of the AuNWs of 6 water dispersible of embodiment
A) 0.308g is weighed, the 3- mercaptopropionic acid of 0.25mmol is dissolved in the solution of 1mL methanol and 0.3mL water,
Adjusting pH value of solution with 40%NaOH solution is 12；
B) measure 5mL 1) in oil-soluble AuNWs solution after purification, 1.3mLa is added) in the mercaptopropionic acid containing 3- mixing
Solution, 37 DEG C of magnetic agitation 30min；
C) 10mL deionized water is added to continue to stir 20min, AuNWs is transferred in water phase by organic phase at this time；
D) lower layer's organic phase is removed, 20mL acetone is added；4000rpm is centrifuged 5min, removes supernatant, and deionized water is added and divides again
It dissipates.
The preparation and purification of the AuNWs of 7 water dispersible of embodiment
A) 0.492g is weighed, the 3- mercaptopropionic acid of 0.4mmol is dissolved in the solution of 1.5mL ethyl alcohol and 1mL water,
Adjusting pH value of solution with 40%NaOH solution is 12；
B) measure 5mL 1) in oil-soluble AuNWs solution after purification, 2.5mLa is added) in the mercaptopropionic acid containing 3- mixing
Solution, 37 DEG C of magnetic agitation 30min；
C) 20mL deionized water is added to continue to stir 20min, AuNWs is transferred in water phase by organic phase at this time；
D) lower layer's organic phase is removed, 20mL acetone is added；4000rpm is centrifuged 5min, removes supernatant, and deionized water is added and divides again
It dissipates.
The preparation and purification of the AuNWs of 8 water dispersible of embodiment
A) 0.106g is weighed, the mercaptoacetic acid solution of 0.1mmol is dissolved in the solution of 1.5mL methanol and 1mL water, is used
It is 12 that 40%NaOH solution, which adjusts pH value of solution,；
B) measure 5mL 1) in oil-soluble AuNWs solution after purification, 2.5mLa is added) in the mercaptopropionic acid containing 3- mixing
Solution, 37 DEG C of magnetic agitation 30min；
C) 10mL deionized water is added to continue to stir 20min, AuNWs is transferred in water phase by organic phase at this time；
D) lower layer's organic phase is removed, 20mL acetone is added；4000rpm is centrifuged 5min, removes supernatant, and deionized water is added and divides again
It dissipates.
The preparation and purification of the AuNWs of 9 water dispersible of embodiment
A) 0.265g is weighed, the mercaptoacetic acid solution of 0.25mmol is dissolved in the solution of 1mL ethyl alcohol and 0.3mL water, is used
It is 12 that 40%NaOH solution, which adjusts pH value of solution,；
B) measure 5mL 1) in oil-soluble AuNWs solution after purification, 1.3mLa is added) in the mercaptopropionic acid containing 3- mixing
Solution, 37 DEG C of magnetic agitation 30min；
C) 10mL deionized water is added to continue to stir 20min, AuNWs is transferred in water phase by organic phase at this time；
D) lower layer's organic phase is removed, 20mL acetone is added；4000rpm is centrifuged 5min, removes supernatant, and deionized water is added and divides again
It dissipates.
The preparation and purification of the AuNWs of 10 water dispersible of embodiment
A) 0.424g is weighed, the mercaptoacetic acid solution of 0.4mmol is dissolved in the solution of 1.5mL methanol and 1mL water, is used
It is 12 that 40%NaOH solution, which adjusts pH value of solution,；
B) measure 5mL 1) in oil-soluble AuNWs solution after purification, 2.5mLa is added) in the mercaptopropionic acid containing 3- mixing
Solution, 37 DEG C of magnetic agitation 30min；
C) 10mL deionized water is added to continue to stir 20min, AuNWs is transferred in water phase by organic phase at this time；
D) lower layer's organic phase is removed, 20mL acetone is added；4000rpm is centrifuged 5min, removes supernatant, and deionized water is added and divides again
It dissipates.
Embodiment 11
The present embodiment is unlike embodiment 5~10: can use hypervelocity concentration in water-soluble AuNWs purification process
Centrifuge tube (interception 10KDa) centrifugation, and other operations are constant, specific steps are by taking embodiment 5 as an example:
A) 0.123g is weighed, the 3- mercaptopropionic acid of 0.1mmol is dissolved in 1mL methanol and 0.3mL water mixed solution
In, adjusting pH value of solution with 40%NaOH solution is 12；
B) measure 5mL 1) in oil-soluble AuNWs solution after purification, 1.3mLa is added) in the mercaptopropionic acid containing 3- mixing
Solution, 37 DEG C of magnetic agitation 30min；
C) 10mL deionized water is added to continue to stir 20min, AuNWs is transferred in water phase by organic phase at this time；
D) lower layer's organic phase is removed, hypervelocity concentration centrifuge tube (interception 10KDa) is added to and is centrifuged, 5500rpm, 6min,
4-5 times, 3- mercaptopropionic acid and other impurities are removed, are dispersed sediment in again in the ultrapure water of certain volume.By sediment
Again it is scattered in the ultrapure water of certain volume, prepares certain density nano wire with subsequent applications.
Illustrating ground is, selects in the temperature of the hydrophilic substitution process of water dispersible AuNWs, if environment temperature is higher,
Room temperature reaction；If environment temperature lower such as winter operates, it is preferably maintained in 37 DEG C of reactions！
The above is only a preferred embodiment of the present invention, it should be pointed out that: for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of water dispersible nanowires of gold, characterized by the following steps:
1) oil-soluble nanowires of gold is prepared
Golden precursor solution is reacted in growth templates molecule, is stood, and solution colour becomes peony from initial yellow, obtains gold
Nanowire suspended liquid；Then nanowires of gold suspension is purified to obtain oil-soluble nanowires of gold；
2) exchange surface hydrophilic ligand
It is exchanged instead with compounds containing thiol groups with the surface hydrophobic oleyl amine functional group of oil-soluble nanowires of gold under strong alkaline condition
It answers, finally obtains water dispersible nanowires of gold after purification.
2. the preparation method of oil-soluble nanowires of gold according to claim 1, it is characterised in that: described in step 1)
Golden precursor solution is HAuCl4Aqueous solution, the growth templates molecule are oleyl amine and n-hexane；By HAuCl4·3H2O dissolution
To completely rear filtering removal insoluble matter in the mixed solution of oleyl amine and n-hexane；Then it is quiet that tri isopropyl silane mixing is added
It sets.
3. the preparation method of oil-soluble nanowires of gold according to claim 2, it is characterised in that: the HAuCl4·
3H2O, oleyl amine, n-hexane reaction molar concentration ratio be 10:(0.2~0.3): (25~50).
4. the preparation method of oil-soluble nanowires of gold according to claim 3, it is characterised in that: the HAuCl4Solution
Concentration be 10mmol/L, the concentration of the tri isopropyl silane is 1mmol/L.
5. the preparation method of oil-soluble nanowires of gold according to claim 1, it is characterised in that: described in step 1)
Purifying are as follows: the dehydrated alcohol of 2~3 times of volumes, piping and druming mixing are added into nanowires of gold suspension, centrifugation is gone after supernatant again
It is scattered in hexane；It repeats purification step 2~3 times.
6. the preparation method of water dispersible nanowires of gold according to claim 1, it is characterised in that: described in step 2)
Compounds containing thiol groups be 3- mercaptopropionic acid or thioacetic acid；3- mercaptopropionic acid or thioacetic acid are weighed, methanol or second are dissolved in
In the aqueous solution of alcohol, adjust pH be 12, be then added into it is above-mentioned be prepared in oil-soluble nanowires of gold solution, magnetic force stirs
Deionized water is added after mixing to continue to stir.
7. the preparation method of water dispersible nanowires of gold according to claim 6, it is characterised in that: described in step 2)
Purifying are as follows: water intaking phase is added acetone soln centrifugation, removes acetone/3- mercaptopropionic acid or thioacetic acid and other impurities, will sink
Starch is scattered in ultrapure water again.
8. the preparation method of water dispersible nanowires of gold according to claim 6, it is characterised in that: described in step 2)
Purifying are as follows: water intaking phase is added to hypervelocity concentration centrifuge tube centrifugation, removes 3- mercaptopropionic acid or thioacetic acid and other impurities,
Again it disperses sediment in ultrapure water.
9. the preparation method of water dispersible nanowires of gold according to claim 6, it is characterised in that: the 3- sulfydryl third
Acid or thioacetic acid and the molar ratio of oil-soluble nanowires of gold solution are (1~4): 1；The methanol or ethyl alcohol and water volume ratio
For 10:(3~6).
10. the preparation method of oil-soluble nanowires of gold according to claim 1, it is characterised in that: in the step 1), institute
The time of repose stated is 24~48h, and reaction temperature is 25 DEG C；In the step 2), reaction temperature is 25~37 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
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