CN101343778A - Process for producing golden nano stick with short length-diameter ratio - Google Patents
Process for producing golden nano stick with short length-diameter ratio Download PDFInfo
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- CN101343778A CN101343778A CNA2008101192465A CN200810119246A CN101343778A CN 101343778 A CN101343778 A CN 101343778A CN A2008101192465 A CNA2008101192465 A CN A2008101192465A CN 200810119246 A CN200810119246 A CN 200810119246A CN 101343778 A CN101343778 A CN 101343778A
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Abstract
The invention discloses a short length-diameter ratio gold nanometer rod preparation method. A strong reducing agent of sodium borohydride is added in a hexadecyl trimethyl ammonium bromide surface modifying agent solution to reduce gold acid chloride and obtain a gold seed solution; a mixed fluid of didodecyl dimethyl ammonium bromide, gold acid chloride and silver nitrate is prepared, and an ascorbic acid solution is added thereto for obtaining a growth solution; the seed solution of a certain amount is filled into the growth solution to react for 5 to 12 hours, so as to obtain the short length-diameter ratio gold nanometer rod. The operation of the method is simple, the gold nanometer rod production rat is high, and the size distribution is narrow.
Description
Technical field
The invention belongs to the nano material preparation technical field, be specifically related to the preparation method of gold nanorods.
Background technology
The physical chemistry of golden nanometer particle and photoelectric property and its pattern and size are closely related, common gold nanorods length-to-diameter ratio is 2-7, because accurate one dimension pattern, the surface plasma body resonant vibration absorption peak is split into two, lateral surfaces plasma resonance absorption peak and a special vertical table surface plasma resonance absorption peak near the 520nm, wherein vertical table surface plasma resonance absorption peak position can be regulated by changing the gold nanorods length-to-diameter ratio, crosses the near-infrared region from visible region.Gold nanorods has special nano-meter characteristic, makes it have broad application prospects in fields such as biomedicine, chemical catalysis, optics, photoelectrons.
The preparation method of gold nanorods mainly contains template, electrochemical process, seed mediated growth method, photochemical method at present.Wherein by Catherine J.Murphy propose (Adv.Mater., 2001,13,1389-1393), Mostafa A.El-Sayed improves (Chem.Mater., 2003,15, seed mediated growth method 1957-1962) is because of the reaction conditions gentleness, and is easy and simple to handle, is used widely.This method adopt usually CTAB (cetyl trimethylammonium bromide) simultaneously as seed solution and coating materials and the shape inducer of growth solution, in the seed growth process, induce reagent to come controlling dimension and shape as pattern by CTAB, can realize regulation and control, thereby realize that its optical property is from the fine adjustments of visible region to near-infrared region gold nanorods length-to-diameter ratio and vertical table surface plasma resonance absorption peak.Yet, in the disclosed seed growth method of above-mentioned document, though CTAB micella environment helps the stability of gold nano-rod particles, but a large amount of existence of CTAB molecule in growth solution have brought some problems: (1) a large amount of CTAB molecules exist at the gold nanorods surface-stable, make the hydrophobization on gold nanorods surface become difficulty [Nikoobakht, B.; EI-Sayed, M.A.Langmuir 2001,17, and 6368]; (2) a large amount of CTAB molecules exist at the gold nanorods surface-stable, make the difficulty more that the bio-modification on gold nanorods surface becomes, and the CTAB molecule has bio-toxicity, have had a strong impact on the application of gold nano-rod particles in biological field like this.
And, be difficult to obtain the gold nanorods with higher yields and distribution of sizes broad of short length-to-diameter ratio (about length-to-diameter ratio 2) according to seed mediated growth method of the prior art.
Thereby this area presses for the preparation method that a kind of high yield high quality golden nano stick with short length-diameter ratio is provided.
The inventor is through long-term conscientious discovering, prepare in the gold nanorods at seed mediated growth method, the CTAB (cetyl trimethylammonium bromide) that routine is prepared in the growth solution of method of gold nanorods uses the two tail base cationic surface modifier didodecyldimethylammbromide bromides (DDAB) of single head base instead, just can solve problems of the prior art, thereby finish the present invention.
Summary of the invention
One object of the present invention is to provide a kind of preparation method of golden nano stick with short length-diameter ratio, and it comprises the steps: 1). the preparation of gold seeds solution; 2). the preparation of growth solution; 3). the growth of gold nanorods; It is characterized in that didodecyldimethylammbromide bromide is added in the growth solution as the growth solution coating materials.
In a preferred scheme of the present invention, it adopts the method for being prepared as follows:
1). the preparation of gold seeds solution: adopt cetyl trimethylammonium bromide finishing agent solution, strong reductant and tetra chlorauric acid to prepare gold seeds solution;
2). the preparation of growth solution: the mixing solutions of preparation didodecyldimethylammbromide bromide, tetra chlorauric acid and Silver Nitrate, wherein the volumetric molar concentration of didodecyldimethylammbromide bromide is 0.004～0.01mol/L, then to wherein adding ascorbic acid solution, vibration shakes up, solution becomes colorless from orange-yellow, promptly obtains growth solution;
3). the growth of gold nanorods: gold seeds solution is injected growth solution react, can obtain the gold nanorods of short length-to-diameter ratio.
In a scheme of the present invention, step 1). described in gold seeds solution in the volumetric molar concentration of cetyl trimethylammonium bromide be 0.05～0.1mol/L, strong reductant and tetra chlorauric acid mol ratio are 1.2.In a preferred embodiment, step 1). in the preparation of gold seeds solution under the stirring at room condition, carry out.
In another scheme of the present invention, step 2). described in the volumetric molar concentration of tetra chlorauric acid solution be 1 * 10
-4～5 * 10
-3Mol/L; Step 3). the gold element mol ratio is 1: 25～100 in middle control gold seeds solution and the growth solution.
In another scheme of the present invention, step 2) mol ratio of xitix and tetra chlorauric acid is 1.5～2.5 in; The mol ratio of Silver Nitrate and tetra chlorauric acid is 0.16～0.4.
In another scheme of the present invention, after step 1) prepares gold seeds solution, this solution is continued to stir 30 minutes, with the unnecessary H that overflows
2
In this article, described strong reductant is sodium borohydride, POTASSIUM BOROHYDRIDE.
In a particularly preferred embodiment of the present invention, the invention provides the preparation method who is prepared as follows golden nano stick with short length-diameter ratio:
1). the preparation of gold seeds solution: under the stirring at room condition, at finite concentration (in 0.05～0.1mol/L) cetyl trimethylammonium bromide (CTAB) the finishing agent solution, reduce tetra chlorauric acid with strong reductant, sodium borohydride and tetra chlorauric acid mol ratio are 1.2, obtain gold seeds solution.Continue to stir the above-mentioned seed solution for preparing 30 minutes, with the unnecessary H that overflows
2
2). the preparation of growth solution: the mixing solutions of preparation DDAB, tetra chlorauric acid and Silver Nitrate, this mixed solution is orange-yellow.The DDAB volumetric molar concentration is 0.004～0.01mol/L in the mixing solutions, and tetra chlorauric acid solution volumetric molar concentration is 1 * 10
-4～5 * 10
-3Mol/L, the mol ratio of Silver Nitrate and tetra chlorauric acid is 0.16～0.4, adds ascorbic acid solution at last in above-mentioned mixed solution, the mol ratio of xitix and tetra chlorauric acid is 1.5～2.5; Vibration shakes up, and solution becomes colorless from orange-yellow, promptly obtains growth solution.
3). the growth of gold nanorods: a certain amount of seed solution is injected growth solution, gold dollar in control seed solution and the growth solution
Plain mol ratio is 1: 25～100, reacts 5～12 hours, promptly obtains the gold nanorods of short length-to-diameter ratio.
Another object of the present invention is to provide the golden nano stick with short length-diameter ratio for preparing according to method of the present invention, and wherein the gold nanorods length-to-diameter ratio is 1.87 ± 0.1, and average major axis is 53 ± 5nm, and average minor axis is 28.3 ± 3nm.
Also purpose of the present invention provides the application of didodecyldimethylammbromide bromide in the preparation golden nano stick with short length-diameter ratio, it is characterized in that in the preparation golden nano stick with short length-diameter ratio, didodecyldimethylammbromide bromide being added in the growth solution as the growth solution coating materials.
In the present invention, if not explanation especially, the device that is adopted, instrument, equipment, material, technology, method etc. all are that this area routine adopts or those of ordinary skills can easily obtain according to the conventional technology that adopts in this area.
In this article, if not explanation especially, the solution that is adopted all prepares under normal condition, such as what at room temperature substance dissolves is prepared in the aqueous solution.
Than the seed mediated growth method of the preparation gold nanorods of available technology adopting, the present invention has following advantage:
1, adopts didodecyldimethylammbromide bromide (DDAB) as the growth solution coating materials, solved the hydrophobization problem and the bio-modification problem that adopt the nanorod surfaces that CTAB brought;
2, coating materials DDAB consumption is little, than low one to two order of magnitude of coating materials cetyl trimethylammonium bromide (CTAB) volumetric molar concentration that routine kind is used in growth solution, has reduced the problem of productive expense and aftertreatment;
The productive rate height of the golden nano stick with short length-diameter ratio that 3, prepares, up to more than 90%, the product distribution of sizes is narrower, length-to-diameter ratio 1.87 ± 0.1.
These advantages have all been improved the character of character, the especially golden nano stick with short length-diameter ratio of gold nanorods greatly, help it and are applied even more extensively.
Description of drawings
The UV, visible light absorption spectrum of the product gold nanorods of Fig. 1 embodiment of the invention 1 preparation;
The transmission electron microscope photo of the product gold nanorods of Fig. 2 embodiment of the invention 1 preparation.
Embodiment
Specifically describe the preparation method of golden nano stick with short length-diameter ratio of the present invention below in conjunction with drawings and Examples, but should be appreciated that these embodiment only are used to set forth the present invention, and also limit protection scope of the present invention never in any form.
The preparation method of golden nano stick with short length-diameter ratio of the present invention realizes as follows:
1). the preparation of gold seeds solution: under the stirring at room condition, be (to add strong reductant solution in 0.05～0.1mol/L) cetyl trimethylammonium bromide and the tetra chlorauric acid mixing solutions in concentration, the mol ratio of control reductive agent and tetra chlorauric acid is 1.2, the volumetric molar concentration of the cetyl trimethylammonium bromide in the mixing solutions is 0.05～0.1mol/L, and the volumetric molar concentration of tetra chlorauric acid is 1 * 10
-4～5 * 10
-3Mol/L, strong reductant reduction tetra chlorauric acid obtains seed solution.Continue to stir the above-mentioned seed solution for preparing 30 minutes, with the unnecessary H that overflows
2
2). the preparation of growth solution: the mixing solutions of preparation DDAB, tetra chlorauric acid and Silver Nitrate, this mixed solution is orange-yellow.The DDAB volumetric molar concentration is 0.004～0.01mol/L in the mixing solutions, and tetra chlorauric acid solution volumetric molar concentration is 1 * 10
-4～5 * 10
-3Mol/L, the mol ratio of Silver Nitrate and tetra chlorauric acid is 0.16～0.4, adds ascorbic acid solution at last in above-mentioned mixed solution, the mol ratio of xitix and tetra chlorauric acid is 1.5～2.5.Vibration shakes up, and solution becomes colorless from orange-yellow, promptly obtains growth solution.
3). the growth of gold nanorods: just a certain amount of seed solution injects growth solution, and the gold element mol ratio is 1: 25～100 in control seed solution and the growth solution, reacts under the room temperature 5～12 hours, promptly obtains the gold nanorods of short length-to-diameter ratio.
Embodiment one
1). the preparation of gold seeds solution:
Under the stirring at room condition, in the mixing solutions of the 0.1mol/L of 10ml cetyl trimethylammonium bromide and 0.0005mol/L tetra chlorauric acid, add abundant refrigerative 0.01mol/LNaBH in 0 ℃ of ice-water bath
4Solution 0.6ml obtains isabelline seed solution after the reaction.Continue to stir the above-mentioned seed solution for preparing 30 minutes, with the unnecessary H that overflows
2
2). the preparation of growth solution: the mixed solution of preparation 10ml DDAB, tetra chlorauric acid and Silver Nitrate in clean reactor, wherein the DDAB volumetric molar concentration is 0.005mol/L, and the volumetric molar concentration of tetra chlorauric acid is 0.0005mol/L, and the Silver Nitrate volumetric molar concentration is 10
-4Mol/L, Silver Nitrate and tetra chlorauric acid mol ratio are 0.2.Add 0.1mol/L ascorbic acid solution 80 μ L at last in mixed solution, control xitix and tetra chlorauric acid mol ratio are 1.6: 1, and vibration shakes up, and solution becomes colorless from orange-yellow, promptly obtains growth solution.
3). the growth of gold nanorods: in above-mentioned steps 2) in add the seed solution that 0.3ml has made in the growth solution of preparation in step 1), the gold element mol ratio that makes seed solution and growth solution is 1: 35, gold nanorods promptly begins to grow.Added the growth solution behind the seed solution and at room temperature reacted 12 hours, obtained gold nanorods, the UV, visible light absorption spectrum of product is seen accompanying drawing 1, and transmission electron microscope photo is seen accompanying drawing 2.As seen, vertical plasma absorption peak of gold nanorods is golden nano stick with short length-diameter ratio near 600nm in the accompanying drawing 1.Referring to the length-to-diameter ratio 1.87 ± 0.1 that the gold nanorods of accompanying drawing more than 2,90% is, average major axis is 53 ± 5nm, and average minor axis is 28.3 ± 3nm, and distribution of sizes is narrower.
Embodiment two
1). the preparation of gold seeds solution: under the stirring at room condition, add abundant refrigerative 0.1mol/L solution of potassium borohydride 0.6ml in 0 ℃ of ice-water bath in the 0.1mol/L of 10ml cetyl trimethylammonium bromide and 0.005mol/L tetra chlorauric acid mixing solutions, reaction obtains isabelline seed solution.Continue to stir seed solution 30 minutes, with the unnecessary H that overflows
2
2). the preparation of growth solution: the mixed solution of preparing 10mlDDAB, tetra chlorauric acid and Silver Nitrate in the clean reactor, the DDAB volumetric molar concentration is 0.01mol/L in the mixing solutions, the volumetric molar concentration of tetra chlorauric acid is 0.005mol/L, the Silver Nitrate volumetric molar concentration is 0.002mol/L, and Silver Nitrate and tetra chlorauric acid mol ratio are 0.4.Add 0.1mol/L ascorbic acid solution 1.25mL at last in mixed solution, control xitix and tetra chlorauric acid mol ratio are 2.5, and vibration shakes up, and solution becomes colorless from orange-yellow, promptly obtains growth solution.
3). the growth of gold nanorods: add the seed solution that 0.1 1ml has made in above-mentioned growth solution, the gold element mol ratio that makes seed solution and growth solution is 1: 96, and gold nanorods promptly begins growth.At room temperature reacted 8 hours, and obtained length-to-diameter ratio and be 1.87 ± 0.1 gold nanorods.
Embodiment three
The first step, the preparation of gold seeds solution: under the stirring at room condition, in 10ml 0.05mol/L cetyl trimethylammonium bromide and 0.0002mol/L tetra chlorauric acid mixing solutions, add abundant refrigerative 0.01mol/L NaBH in 0 ℃ of ice-water bath
4Solution 0.24ml, control sodium borohydride and tetra chlorauric acid mol ratio are 1.2: 1, reaction obtains isabelline seed solution.So the seed solution of preparation continues to stir 30 minutes, with the unnecessary H that overflows
2
Second step, the preparation of growth solution: preparation 10ml mixed solution in the clean reactor, wherein the didodecyldimethylammbromide bromide volumetric molar concentration is 0.004mol/L, and the tetra chlorauric acid volumetric molar concentration is 0.0002mol/L, and the Silver Nitrate volumetric molar concentration is 3.2 * 10
-5Mol/L, Silver Nitrate and tetra chlorauric acid mol ratio are 0.16.Add 0.1mol/L ascorbic acid solution 40 μ L at last, control xitix and tetra chlorauric acid mol ratio are 2: 1, and vibration shakes up, and solution becomes colorless from orange-yellow, promptly obtains growth solution.
In the 3rd step, the growth of gold nanorods: add the seed solution that 0.4ml has made in above-mentioned growth solution, the gold element mol ratio that makes seed solution and growth solution is 1: 25.6, and gold nanorods promptly begins growth.This growth solution at room temperature reacted 5 hours, obtained the gold nanorods of length-to-diameter ratio 1.87 ± 0.1.
Embodiment four
The first step, the preparation of gold seeds solution: under the stirring at room condition, in 10ml 0.08mol/L cetyl trimethylammonium bromide and 0.0005mol/L tetra chlorauric acid mixing solutions, add abundant refrigerative 0.01mol/L NaBH in 0 ℃ of ice-water bath
4Solution 0.6ml, control sodium borohydride and tetra chlorauric acid mol ratio are 1.2: 1, reaction obtains isabelline seed solution.So the seed solution of preparation continues to stir 30 minutes, with the unnecessary H that overflows
2
Second step, the preparation of growth solution: preparation 10ml mixed solution in the clean reactor, wherein the didodecyldimethylammbromide bromide volumetric molar concentration is 0.006mol/L, and the tetra chlorauric acid volumetric molar concentration is 0.0005mol/L, and the Silver Nitrate volumetric molar concentration is 10
-4Mol/L.Add 0.1mol/L ascorbic acid solution 90 μ L at last, control xitix and tetra chlorauric acid mol ratio are 1.8: 1, and vibration shakes up, and solution becomes colorless from orange-yellow, promptly obtains growth solution.
In the 3rd step, the growth of gold nanorods: add the seed solution that 0.35ml has made in above-mentioned growth solution, the gold element mol ratio that makes seed solution and growth solution is 1: 30, and gold nanorods promptly begins growth.This growth solution at room temperature reacted 10 hours, obtained the gold nanorods of length-to-diameter ratio 1.87 ± 0.1.
Embodiment five
The first step, the preparation of gold seeds solution: under the stirring at room condition, in 10ml 0.08mol/L CTAB and 0.001mol/L tetra chlorauric acid mixing solutions, add abundant refrigerative 0.02mol/LNaBH4 solution 0.6ml in 0 ℃ of ice-water bath, the reduction tetra chlorauric acid, reaction obtains isabelline seed solution.Continue to stir the above-mentioned seed solution for preparing 30 minutes, with the unnecessary H2 that overflows.
In second step, the preparation of growth solution: prepare the mixed solution of 10mlDDAB, tetra chlorauric acid and Silver Nitrate in the clean reactor, wherein the DDAB volumetric molar concentration is 0.006mol/L, and the volumetric molar concentration of tetra chlorauric acid is 0.0008mol/L, and the Silver Nitrate volumetric molar concentration is 2 * 10
-4Mol/L, Silver Nitrate and tetra chlorauric acid mol ratio are 0.25.Add 0.1mol/L ascorbic acid solution 144 μ L at last in mixed solution, xitix and tetra chlorauric acid mol ratio are 1.8, and vibration shakes up, and solution becomes colorless from orange-yellow, promptly obtains growth solution.
In the 3rd step, the growth of gold nanorods: add the seed solution that 0.2ml has made in the growth solution of preparation in the first step in above-mentioned second step, the gold element mol ratio that makes seed solution and growth solution is 1: 42, and gold nanorods promptly begins growth.Add the growth solution behind the seed solution and at room temperature reacted 10 hours, obtained length-to-diameter ratio 1.87 ± 0.1 gold nanorods.
Claims (9)
1, the preparation method of golden nano stick with short length-diameter ratio, it comprises the steps:
1). the preparation of gold seeds solution: adopt cetyl trimethylammonium bromide finishing agent solution, strong reductant and tetra chlorauric acid to prepare gold seeds solution;
2). the preparation of growth solution: the mixing solutions of preparation didodecyldimethylammbromide bromide, tetra chlorauric acid and Silver Nitrate, wherein the volumetric molar concentration of didodecyldimethylammbromide bromide is 0.004～0.01mol/L, then to wherein adding ascorbic acid solution, vibration shakes up, solution becomes colorless from orange-yellow, promptly obtains growth solution;
3). the growth of gold nanorods: gold seeds solution is injected growth solution react, can obtain the gold nanorods of short length-to-diameter ratio.
2, the preparation method of golden nano stick with short length-diameter ratio according to claim 1, wherein step 1). described in gold seeds solution in the volumetric molar concentration of cetyl trimethylammonium bromide be 0.05～0.1mol/L, strong reductant and tetra chlorauric acid mol ratio are 1.2.
3, the preparation method of golden nano stick with short length-diameter ratio according to claim 1 and 2, wherein said strong reductant is POTASSIUM BOROHYDRIDE, sodium borohydride.
4, the preparation method of golden nano stick with short length-diameter ratio according to claim 1 and 2, the volumetric molar concentration of wherein said tetra chlorauric acid solution are 1 * 10
-4～5 * 10
-3Mol/L; Step 3). the gold element mol ratio is 1: 25～100 in middle control seed solution and the growth solution.
5, the preparation method of the golden nano stick with short length-diameter ratio of claim 1, wherein step 2) in the mol ratio of xitix and tetra chlorauric acid be 1.5～2.5; The mol ratio of Silver Nitrate and tetra chlorauric acid is 0.16～0.4.
6, the preparation method of golden nano stick with short length-diameter ratio according to claim 1 and 2, wherein the reaction times in the step 3) is 5～12 hours.
7, the preparation method of golden nano stick with short length-diameter ratio according to claim 1 and 2 wherein after step 1) prepares gold seeds solution, continues this solution to stir 30 minutes.
8, the application of didodecyldimethylammbromide bromide in the preparation golden nano stick with short length-diameter ratio is characterized in that in the preparation golden nano stick with short length-diameter ratio didodecyldimethylammbromide bromide being added in the growth solution as the growth solution coating materials.
9, the golden nano stick with short length-diameter ratio for preparing according to each method among the claim 1-8, wherein the gold nanorods length-to-diameter ratio is 1.87 ± 0.1, and average major axis is 53 ± 5nm, and average minor axis is 28.3 ± 3nm.
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