CN112809018A - Synthesis method of gold-platinum bimetallic structure material - Google Patents

Synthesis method of gold-platinum bimetallic structure material Download PDF

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CN112809018A
CN112809018A CN202011637855.7A CN202011637855A CN112809018A CN 112809018 A CN112809018 A CN 112809018A CN 202011637855 A CN202011637855 A CN 202011637855A CN 112809018 A CN112809018 A CN 112809018A
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CN112809018B (en
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邓天松
张棋
卫鸣璋
顾伊杰
程知群
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Hangzhou Dianzi University
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Abstract

The invention discloses a method for synthesizing a gold-platinum bimetallic structure material, wherein the bimetallic structure comprises a gold nanorod serving as a core structure and platinum serving as a shell structure. The invention adopts a seed growth method to grow platinum on the gold nanorods. The method mainly comprises the following steps: firstly, growing gold nanorods by using a seed growth method, and then cleaning the successfully grown gold nanorods to obtain gold nanorods with higher purity; then, taking the gold nanorods as seeds, adding a corresponding amount of surfactant, platinate and reducing agent, and uniformly mixing; and finally, controlling the reaction temperature to ensure that platinum is successfully grown on the gold nanorods, and observing the growth condition of the platinum by a transmission electron microscope image. The gold-platinum bimetal synthesized by the method is more uniform, the reaction conditions are simpler, the reaction speed is improved, and the low cost is realized.

Description

Synthesis method of gold-platinum bimetallic structure material
Technical Field
The invention relates to the field of synthesis of metal nano materials, in particular to a synthesis method of a gold-platinum bimetallic structure material.
Background
Research on noble metal nanoparticles has been rapidly developed in recent years, with gold nanorods being the most prominent. Since gold nanorods have very abundant chemical and physical properties, first it can be used in life sciences including in vitro diagnostics, in vivo imaging and in vivo therapy. Secondly, gold nanorods are also widely used in the sensor field, and can be used for trace molecule and ion detection due to the gold nanorods have extremely strong surface raman scattering enhancement and surface plasmon resonance performance. Meanwhile, the gold nanorods can also be made into optical elements, such as: near infrared filters, solar cells, polarizers, and the like. Besides, the gold nanorods also have an important application-being widely applied to the field of catalysis, namely, under the same temperature and chemical and physical environment, the platinum-coated gold nanorods can have higher catalytic activity than a single platinum catalyst with the same dosage, and simultaneously have better stability. The catalytic performance of the catalyst is particularly remarkable for the photothermal conversion characteristic, on one hand, the catalyst can provide temperature activation on the surface of the nano particles, and on the other hand, the catalyst can save energy required by heating the whole solution system. Therefore, how to synthesize the catalyst with the bimetallic structure efficiently becomes the focus of researchers.
When researching the catalyst with the bimetallic structure, researchers find that the gold-platinum bimetallic structure has more efficient catalytic performance. Therefore, the research on the synthesis of the gold-platinum bimetallic structure is essential. The existing synthesis method has the defects of long synthesis time, more complicated method, uneven synthesized bimetal structure and the like. How to synthesize a uniform gold-platinum bimetallic structure efficiently is a problem to be solved at present.
Disclosure of Invention
In order to solve the problems of long synthesis time and non-uniform synthesis of the gold-platinum bimetal, the invention provides a synthesis method of a gold-platinum bimetal structural material, which can efficiently synthesize a uniform gold-platinum bimetal structure and has the advantages of simple reaction conditions and low cost.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme:
a synthetic method of a gold-platinum bimetal structural material comprises the following steps:
and step S1, preparing the gold nanorods by using a seed growth method.
Step S2, taking gold nanorods which are cleaned and dispersed in low-concentration CTAB as new seeds, adding corresponding amounts of CTAC, silver nitrate solution, potassium tetrachloroplatinate solution and ascorbic acid solution on the seeds, and controlling the reaction temperature to synthesize the bimetallic structure.
Wherein the step S1 further includes the following steps:
s10 mixing 10mL CTAB (0.1M) and 0.25mL HAuCl4(10mM) are mixed in a bottle with an ice-water mixture and a weighed quantity of NaBH4Mix to make 0.01M solution, and add 0.6mL into the bottle and stir vigorously. The solution changed from golden yellow to brown yellow, which is a seed solution.
S11 2.5mL CTAB (0.1M) and 0.037g NaOL were dissolved in 21.25mL of water at 50 ℃. After dissolution, the solution was cooled to 30 ℃ and then 0.9mL of AgNO was added3(4mM) solution. And left to stand at a constant temperature of 30 ℃ for 15 minutes, after which 0.25mL of HAuCl was added4(10 mM). After stirring (400rpm) for 60-90 minutes, the solution turned from golden yellow to colorless. This is the growth solution.
S12 pH was adjusted by adding 0.3mL HCl (37 wt.%) to the growth solution. Then 75. mu.L of AA (64mM), 40. mu.L of the seed solution were added in succession and stirred vigorously. The final solution was left to stand for 12 hours in a 30 ℃ water bath.
S13 the solution after growth was centrifuged (7000rpm, 30 minutes), the supernatant removed and CTAB (1-2mM) added, followed by a second centrifugation (7000rpm, 30 minutes). After removal of the supernatant, it was dispersed in a corresponding volume of CTAB (1-2 mM).
The step S2 further includes the steps of:
s20 gold nanorods dispersed in CTAB (1 mL) were taken out and put in a bottle, and CTAC (34mL 30mM), silver nitrate solution (0.5mL 4mM), potassium tetrachloroplatinate solution (0.5mL 2mM), and ascorbic acid solution (0.5mL 100mM) were added in this order and stirred with a magnetic stirrer (400rpm) for 2 minutes to mix them uniformly.
S21: the solution was placed in a water bath at 60 ℃ and heated for 30 minutes. After 30 minutes, it was removed.
S22: the final product obtained above was centrifuged (7000rpm, 30 minutes), the supernatant removed and CTAB (1-2mM) added, followed by a second centrifugation (7000rpm, 30 minutes). And (4) preparing a transmission electron microscope sample, and observing the successfully synthesized gold-platinum bimetallic structure.
As a further improvement, the step S2 is carried out under the water bath heating condition of 60 ℃, and the reducing agent ascorbic acid is added to reduce bivalent platinum ions in potassium tetrachloroplatinate on the gold nanorods, so that the reaction time is greatly shortened, and the gold-platinum bimetal can be obtained within half an hour.
In the technical scheme of the invention, the synthesis is carried out by adopting a seed growth method, and the whole process can be divided into two parts. In the first part, a seed growing method is firstly utilized to successfully synthesize uniform gold nanorods. And then taking the cleaned gold nanorods as seeds, adding a surfactant CTAC, a silver nitrate solution, a potassium tetrachloroplatinate solution and ascorbic acid, and heating for 30 minutes in a water bath at 60 ℃ to finally obtain uniform gold-platinum bimetal. The reason why the reaction is carried out in a 60 ℃ water bath is that the bimetal structure can grow uniformly; the addition of the reducing agent ascorbic acid is due to the fact that ascorbic acid greatly increases the rate of reaction. Therefore, the method can be used for efficiently synthesizing a uniform gold-platinum bimetallic structure, and has the advantages of simple reaction conditions and low cost.
The invention synthesizes a material with a special structure of a gold-platinum bimetallic structure, which takes a gold nanorod as a core and platinum as a shell, and platinum uniformly grows on the gold nanorod. The surface of the finally synthesized gold-platinum bimetal structure presents a granular shape, and the synthesized bimetal has the characteristic of uniformity.
As a further improvement, the material is prepared by the material of claim 1, wherein, the gold nanorods which have been successfully grown are used as seeds, and the growth condition of the gold-platinum bimetallic structure is controlled by controlling the amount of platinate; the time required for the reaction was greatly shortened by changing the conventional surfactant, using CTAC and adding AA. And finally, Pt grows on the gold nanorods to form a bimetal structure.
The invention synthesizes a material with a gold-platinum bimetallic structure, and has the following beneficial effects:
(1) the synthesized gold-platinum bimetallic structure does not completely change the performance of the gold nanorods, but retains the special properties of the gold nanorods.
(2) The uniform growth of the gold-platinum bimetallic structure enhances the catalytic performance of the gold nanorods, and the bimetallic structure can enhance the catalytic activity and realize the effect of lower energy.
(3) The synthesis method of the bimetal structure is simple, and the finally obtained product gold-platinum is very stable and has extremely high reliability.
(4) The gold-platinum bimetallic structure has some special properties of both gold and platinum, and thus can be applied more widely. For example: biomedicine, optical catalysis, etc.
Drawings
FIG. 1 is a flow chart of the steps for the synthesis of a gold-platinum bimetallic structural material of the present invention;
fig. 2 is a transmission electron microscope image of the gold-platinum bimetallic structural material of example 1 of the present invention.
Detailed Description
The technical solution provided by the present invention will be further explained with reference to the accompanying drawings.
The gold nanorods have good physical and chemical properties, surface plasmon resonance performance and can be widely applied to the field of catalysis, especially photo-thermal conversion. Therefore, the prepared gold nanorods are used as seeds, and platinum grows on the surfaces of the gold nanorods to form a bimetal structure. The gold-platinum bimetallic structure is a composite catalyst, can greatly enhance the catalytic efficiency, has higher catalytic activity and has higher stability. Therefore, the invention provides a synthesis method of a gold-platinum bimetallic structure material.
Referring to fig. 1, the synthesis method of the gold-platinum bimetallic structure provided by the invention specifically comprises the following steps:
and step S1, preparing the gold nanorods by using a seed growth method.
Step S2, taking gold nanorods which are cleaned and dispersed in low-concentration CTAB as new seeds, adding corresponding amounts of CTAC, silver nitrate solution, potassium tetrachloroplatinate solution and ascorbic acid solution on the seeds, and controlling the reaction temperature to synthesize the bimetallic structure.
Wherein the step S1 further includes the following steps:
s10 mixing 10mL CTAB (0.1M) and 0.25mL HAuCl4(10mM) are mixed in a bottle with an ice-water mixture and a weighed quantity of NaBH4Mix to make 0.01M solution, and add 0.6mL into the bottle and stir vigorously. The solution changed from golden yellow to brown yellow, which is a seed solution.
S11 2.5mL CTAB (0.1M) and 0.037g NaOL were dissolved in 21.25mL of water at 50 ℃. After dissolution the solution was cooled to 30 ℃ after which 0.9mL of AgNO3(4mM) solution was added. And left to stand at a constant temperature of 30 ℃ for 15 minutes, after which 0.25mL of HAuCl was added4(10 mM). After stirring (400rpm) for 60-90 minutes, the solution turned from golden yellow to colorless. This is the growth solution.
S12 pH was adjusted by adding 0.3mL HCl (37 wt.%) to the growth solution. Then 75. mu.L of AA (64mM), 40. mu.L of the seed solution were added in succession and stirred vigorously. The final solution was left to stand for 12 hours in a 30 ℃ water bath.
S13 the solution after growth was centrifuged (7000rpm, 30 minutes), the supernatant removed and CTAB (1-2mM) added, followed by a second centrifugation (7000rpm, 30 minutes). After removal of the supernatant, it was dispersed in a corresponding volume of CTAB (1-2 mM).
The step S2 further includes the steps of:
s20 gold nanorods dispersed in CTAB (1 mL) were taken out and put in a bottle, and CTAC (34mL 30mM), silver nitrate solution (0.5mL 4mM), potassium tetrachloroplatinate solution (0.5mL 2mM), and ascorbic acid solution (0.5mL 100mM) were added in this order and stirred with a magnetic stirrer (400rpm) for 2 minutes to mix them uniformly.
S21: the solution was placed in a 60 ℃ water bath and heated for 30 minutes. After 30 minutes, it was removed.
S22: the final product obtained above was centrifuged (7000rpm, 30 minutes), the supernatant removed and CTAB (1-2mM) added, followed by a second centrifugation (7000rpm, 30 minutes). And (4) preparing a transmission electron microscope sample, and observing the successfully synthesized gold-platinum bimetallic structure.
The existing synthesis method has the defects that the temperature is higher than that adopted by the method, the finally grown platinum is quite uneven, and the reaction time is long. In the method, the reaction time is greatly shortened, and meanwhile, platinum is uniformly deposited on the gold nanorods, and the finally obtained product, namely a uniform gold-platinum bimetallic structure can reach 99%. Referring to fig. 2, a transmission electron micrograph is shown, in which the reaction efficiency is improved by adding ascorbic acid under the condition of 60 ℃, and the final Pt grows more uniformly on the surface of the gold nanorod. That is, fig. 2 is a transmission electron microscope image of the gold-platinum bimetallic structure finally prepared by the invention. As can be seen, the Au-Pt bimetallic surface appears granular, with a length of about 105nm, a diameter of 25nm, and an aspect ratio of 4.2. Meanwhile, as can be seen from the figure, the gold-platinum bimetal grows uniformly, the two ends grow thicker, the side grows thinner, the stability of the bimetal can be greatly enhanced, and the bimetal has the excellent performances of gold and platinum.
Example 1:
10mL CTAB (0.1M) and 0.25mL HAuCl4(10mM) are mixed in a bottle with an ice-water mixture and a weighed quantity of NaBH4Mix to make 0.01M solution, and add 0.6mL into the bottle and stir vigorously. The solution changed from golden yellow to brown yellow, which is a seed solution. 2.5mL CTAB (0.1M) and 0.037g NaOL were dissolved in 21.25mL of water at 50 ℃. After dissolution, the solution was cooled to 30 ℃ and then 0.9mL of AgNO was added3(4mM) solution. And left to stand at a constant temperature of 30 ℃ for 15 minutes, after which 0.25mL of HAuCl was added4(10 mM). After stirring (400rpm) for 60-90 minutes, the solution turned from golden yellow to colorless. This is the growth solution. To the growth solution was added 0.3mL HCl (37 wt.%) to adjust the pH. Then 75. mu.L of AA (64mM), 40. mu.L of the seed solution were added in succession and stirred vigorously. The final solution was left to stand for 12 hours in a 30 ℃ water bath. The solution after growth was centrifuged (7000rpm, 30 minutes), the supernatant removed and CTAB (1-2mM) added, and centrifuged a second time (7000rpm, 30 minutes). After removal of the supernatant, it was dispersed in a corresponding volume of CTAB (1-2 mM). 1mL of gold nanorods dispersed in CTAB were taken out of a bottle, and CTAC (34mL of 30mM), a silver nitrate solution (0.5mL of 4mM), a potassium tetrachloroplatinate solution (0.5mL of 2mM), and an ascorbic acid solution (0.5mL of 100mM) were added in this order and stirred with a magnetic stirrer (400rpm) for 2 minutes to mix them uniformly. The solution was then placed in a water bath at 60 ℃ and heated for 30 minutes, after which it was removed after 30 minutes. The final product obtained above was centrifuged (7000rpm, 30 minutes), the supernatant removed and CTAB (1-2mM) added, followed by a second centrifugation (7000rpm, 30 minutes). And (4) preparing a transmission electron microscope sample, and observing the successfully synthesized gold-platinum bimetallic structure.
Example 2:
10mL CTAB (0.1M) and 0.25mL HAuCl4(10mM) are mixed in a bottle with an ice-water mixture and a weighed quantity of NaBH4Mix to make 0.01M solution, and add 0.6mL into the bottle and stir vigorously. The solution changed from golden yellow to brown yellow, which is a seed solution. 2.5mL CTAB (0.1M) and 0.037g NaOL were dissolved in 21.25mL of water at 50 ℃. After dissolution, the solution was cooled to 30 ℃ and then 0.9mL of AgNO was added3(4mM) solution. And left to stand at a constant temperature of 30 ℃ for 15 minutes, after which 0.25mL of HAuCl was added4(10 mM). After stirring (400rpm) for 60-90 minutes, the solution turned from golden yellow to colorless. This is the growth solution. To the growth solution was added 0.3mL HCl (37 wt.%) to adjust the pH. Then 75. mu.L of AA (64mM), 40. mu.L of the seed solution were added in succession and stirred vigorously. The final solution was left to stand for 12 hours in a 30 ℃ water bath. The solution after growth was centrifuged (7000rpm, 30 minutes), the supernatant removed and CTAB (1-2mM) added, and centrifuged a second time (7000rpm, 30 minutes). After removal of the supernatant, it was dispersed in a corresponding volume of CTAB (1-2 mM). 0.5mL of gold nanorods dispersed in CTAB were taken out of a bottle, and CTAC (17mL of 30mM), a silver nitrate solution (0.25mL of 4mM), a potassium tetrachloroplatinate solution (0.25mL of 2mM), and an ascorbic acid solution (0.25mL of 100mM) were added in this order and stirred with a magnetic stirrer (400rpm) for 2 minutes to mix them uniformly. Then placing the solution inThe mixture was heated in a water bath at 60 ℃ for 30 minutes and then taken out after 30 minutes. The final product obtained above was centrifuged (7000rpm, 30 minutes), the supernatant removed and CTAB (1-2mM) added, followed by a second centrifugation (7000rpm, 30 minutes). And (4) preparing a transmission electron microscope sample, and observing the successfully synthesized gold-platinum bimetallic structure.
Example 3:
10mL CTAB (0.1M) and 0.25mL HAuCl4(10mM) are mixed in a bottle with an ice-water mixture and a weighed quantity of NaBH4Mix to make 0.01M solution, and add 0.6mL into the bottle and stir vigorously. The solution changed from golden yellow to brown yellow, which is a seed solution. 2.5mL CTAB (0.1M) and 0.037g NaOL were dissolved in 21.25mL of water at 50 ℃. After dissolution the solution was cooled to 30 ℃ after which 0.9mL of AgNO3(4mM) solution was added. And left to stand at a constant temperature of 30 ℃ for 15 minutes, after which 0.25mL of HAuCl was added4(10 mM). After stirring (400rpm) for 60-90 minutes, the solution turned from golden yellow to colorless. This is the growth solution. To the growth solution was added 0.3mL HCl (37 wt.%) to adjust the pH. Then 75. mu.L of AA (64mM), 40. mu.L of the seed solution were added in succession and stirred vigorously. The final solution was left to stand for 12 hours in a 30 ℃ water bath. The solution after growth was centrifuged (7000rpm, 30 minutes), the supernatant removed and CTAB (1-2mM) added, and centrifuged a second time (7000rpm, 30 minutes). After removal of the supernatant, it was dispersed in a corresponding volume of CTAB (1-2 mM). 2mL of gold nanorods dispersed in CTAB were taken out of a bottle, and CTAC (68mL of 30mM), a silver nitrate solution (1mL of 4mM), a potassium tetrachloroplatinate solution (1mL of 2mM), and an ascorbic acid solution (1mL of 100mM) were added in this order and stirred with a magnetic stirrer (400rpm) for 2 minutes to mix them uniformly. The solution was then placed in a water bath at 60 ℃ and heated for 30 minutes, after which it was removed after 30 minutes. The final product obtained above was centrifuged (7000rpm, 30 minutes), the supernatant removed and CTAB (1-2mM) added, followed by a second centrifugation (7000rpm, 30 minutes). And (4) preparing a transmission electron microscope sample, and observing the successfully synthesized gold-platinum bimetallic structure.
Example 4:
10mL CTAB (0.1M) and 0.25mL HAuCl4(10mM) are mixed in a bottle with an ice-water mixture and a weighed quantity of NaBH4Mixing and preparing0.01M solution, and 0.6mL was added to the flask and stirred vigorously. The solution changed from golden yellow to brown yellow, which is a seed solution. 2.5mL CTAB (0.1M) and 0.037g NaOL were dissolved in 21.25mL of water at 50 ℃. After dissolution the solution was cooled to 30 ℃ after which 0.9mL of AgNO3(4mM) solution was added. And left to stand at a constant temperature of 30 ℃ for 15 minutes, after which 0.25mL of HAuCl was added4(10 mM). After stirring (400rpm) for 60-90 minutes, the solution turned from golden yellow to colorless. This is the growth solution. To the growth solution was added 0.3mL HCl (37 wt.%) to adjust the pH. Then 75. mu.L of AA (64mM), 40. mu.L of the seed solution were added in succession and stirred vigorously. The final solution was left to stand for 12 hours in a 30 ℃ water bath. The solution after growth was centrifuged (7000rpm, 30 minutes), the supernatant removed and CTAB (1-2mM) added, and centrifuged a second time (7000rpm, 30 minutes). After removal of the supernatant, it was dispersed in a corresponding volume of CTAB (1-2 mM). 0.8mL of gold nanorods dispersed in CTAB were taken out of a flask, and CTAC (27.2mL of 30mM), a silver nitrate solution (0.4mL of 4mM), a potassium tetrachloroplatinate solution (0.4mL of 2mM), and an ascorbic acid solution (0.4mL of 100mM) were added in this order and stirred with a magnetic stirrer (400rpm) for 2 minutes to mix them uniformly. The solution was then placed in a water bath at 60 ℃ and heated for 30 minutes, after which it was removed after 30 minutes. The final product obtained above was centrifuged (7000rpm, 30 minutes), the supernatant removed and CTAB (1-2mM) added, followed by a second centrifugation (7000rpm, 30 minutes). And (4) preparing a transmission electron microscope sample, and observing the successfully synthesized gold-platinum bimetallic structure.
Example 5:
10mL CTAB (0.1M) and 0.25mL HAuCl4(10mM) are mixed in a bottle with an ice-water mixture and a weighed quantity of NaBH4Mix to make 0.01M solution, and add 0.6mL into the bottle and stir vigorously. The solution changed from golden yellow to brown yellow, which is a seed solution. 2.5mL CTAB (0.1M) and 0.037g NaOL were dissolved in 21.25mL of water at 50 ℃. After dissolution, the solution was cooled to 30 ℃ and then 0.9mL of AgNO was added3(4mM) solution. And left to stand at a constant temperature of 30 ℃ for 15 minutes, after which 0.25mL of HAuCl was added4(10 mM). After stirring (400rpm) for 60-90 minutes, the solution turned from golden yellow to colorless. This is the growth solution. To the growth solution was added 0.3mL HCl (37 wt.%) to adjust the pH. Then in turnAdd 75. mu.L of AA (64mM), 40. mu.L of seed solution and stir vigorously. The final solution was left to stand for 12 hours in a 30 ℃ water bath. The solution after growth was centrifuged (7000rpm, 30 minutes), the supernatant removed and CTAB (1-2mM) added, and centrifuged a second time (7000rpm, 30 minutes). After removal of the supernatant, it was dispersed in a corresponding volume of CTAB (1-2 mM). 0.6mL of gold nanorods dispersed in CTAB were taken out of a flask, and CTAC (20.4mL of 30mM), a silver nitrate solution (0.3mL of 4mM), a potassium tetrachloroplatinate solution (0.3mL of 2mM), and an ascorbic acid solution (0.3mL of 100mM) were added in this order and stirred with a magnetic stirrer (400rpm) for 2 minutes to mix them uniformly. The solution was then placed in a water bath at 60 ℃ and heated for 30 minutes, after which it was removed after 30 minutes. The final product obtained above was centrifuged (7000rpm, 30 minutes), the supernatant removed and CTAB (1-2mM) added, followed by a second centrifugation (7000rpm, 30 minutes). And (4) preparing a transmission electron microscope sample, and observing the successfully synthesized gold-platinum bimetallic structure.
Finally, it should be noted that the above embodiments are only used to help understand the method of the present invention and its core idea, and not to limit it. Those of ordinary skill in the art will understand that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications or substitutions do not depart from the spirit and scope of the present invention's device solution. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (4)

1. A synthetic method of a gold-platinum bimetal structural material is characterized by comprising the following steps:
step S1, preparing gold nanorods by using a seed growth method;
step S2, taking gold nanorods which are cleaned and dispersed in low-concentration Cetyl Trimethyl Ammonium Bromide (CTAB) as new seeds, adding corresponding amounts of CTAC, silver nitrate solution, potassium tetrachloroplatinate solution and ascorbic acid solution on the seeds, and controlling the reaction temperature to synthesize a bimetallic structure;
wherein the step S1 further includes the following steps:
s10 mixing 10mL of 0.1M CTAB with 0.25mL of 10mM HAuCl4Mixing in a bottle, mixing with ice-water mixture and certain weighed NaBH4Mixing to prepare 0.01M solution, and adding 0.6mL of the solution into a bottle for vigorous stirring; the solution turns from golden yellow to brown yellow, which is a seed solution;
s11 dissolving 2.5mL of 0.1M CTAB and 0.037g of NaOL in 21.25mL of water at 50 ℃; after dissolution, the solution was cooled to 30 ℃ and then 0.9mL of 4mM AgNO3 solution was added; and left to stand at a constant temperature of 30 ℃ for 15 minutes, after which 0.25mL of 10mM HAuCl was added4(ii) a After stirring at 400rpm for 60-90 minutes, the solution turns from golden yellow to colorless; this is the growth solution;
s12, adding 0.3mL of 37 wt.% HCl into the growth solution to regulate the pH value; then 75 μ L of 64mM AA, 40 μ L of seed solution are added in turn and stirred vigorously; standing the final solution for 12 hours in a water bath at 30 ℃;
s13, 7000rpm of the solution after growth is centrifuged for 30 minutes, 1-2mM CTAB is added after supernatant liquid is removed, 7000rpm is carried out twice, and centrifugation is carried out for 30 minutes; after removing the clear solution, dispersing in a corresponding volume of 1-2mM CTAB;
the step S2 further includes the steps of:
s20, putting 1mL of gold nanorods dispersed in CTAB into a bottle, and sequentially adding 34mL of 30mM CTAC, 0.5mL of 4mM silver nitrate solution, 0.5mL of 2mM potassium tetrachloroplatinate solution and 0.5mL of 100mM ascorbic acid solution, stirring for 2 minutes at 400rpm of a magnetic stirrer, and uniformly mixing;
s21: placing the solution in a water bath at 60 ℃ and heating for 30 minutes; taking out after 30 minutes;
s22: 7000rpm of the final product obtained above is centrifuged for 30 minutes, 1-2mM CTAB is added after supernatant liquid is removed, and 7000rpm is centrifuged for two times for 30 minutes; and (4) preparing a transmission electron microscope sample, and observing the successfully synthesized gold-platinum bimetallic structure.
2. The method for synthesizing a gold-platinum bimetallic structural material as in claim 1, wherein the step S2 is performed under the water bath heating condition of 60 ℃, and the divalent platinum ions in potassium tetrachloroplatinate are reduced on the gold nanorods by adding ascorbic acid as a reducing agent, thereby obtaining the gold-platinum bimetallic.
3. The method for synthesizing a gold-platinum bimetallic structural material as claimed in claim 1, characterized in that the growth of the gold-platinum bimetallic structure is controlled by controlling the amount of platinate by using the gold nanorods that have been successfully grown as seeds; CTAC was used and the time required for the reaction was greatly shortened by adding AA; and finally, Pt grows on the gold nanorods to form a bimetal structure.
4. The method for synthesizing a gold-platinum bimetallic structural material as in claim 3, wherein the gold-platinum bimetallic has a length of 105nm, a diameter of 25nm and an aspect ratio of 4.2.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113500199A (en) * 2021-06-10 2021-10-15 浙江大学 Preparation method of gold-platinum-based bimetallic active oxygen self-generating nano material, product and application thereof
CN115998865A (en) * 2022-12-27 2023-04-25 山东大学 Platinum-gold nanorod@MOF composite material and preparation method and application thereof

Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101450380A (en) * 2007-12-03 2009-06-10 国家纳米科学中心 Bimetal nano rod of branched gold core/platinum shell structure and preparation method thereof
CN101623762A (en) * 2008-07-09 2010-01-13 国家纳米科学中心 Island-shaped porous tri-metal nano rod with gold core/silver-platinum alloy shell structure and method for preparing same
CN101992294A (en) * 2009-08-19 2011-03-30 三星电机株式会社 Method for preparing metal nanoparticles using matal seed and metal nanoparticles comprising metal seed
US20110278497A1 (en) * 2010-05-11 2011-11-17 China Medical University Nanometal dispersion and method for preparing the same
CN106862581A (en) * 2015-12-10 2017-06-20 济南大学 A kind of concave surface gold@silver platinum Heterogeneous Composite nano-particles with superior catalytic and absorbing properties and preparation method thereof
KR101767342B1 (en) * 2016-07-29 2017-08-10 성균관대학교산학협력단 Multi block nanorods and method fabricating thereof
KR20180019888A (en) * 2016-08-17 2018-02-27 한림대학교 산학협력단 Gold multipod nanoparticle core-platinium shell nanoparticles and synthetic method thereof
WO2018069646A1 (en) * 2016-10-13 2018-04-19 Universite Paris Diderot Synthesis of core-shell nanoparticles and uses of said nanoparticles for surface-enhanced raman spectroscopy
CN108031840A (en) * 2018-01-15 2018-05-15 国家纳米科学中心 A kind of heterogeneous nano-superstructure of self-supporting metal and its preparation method and application
CN108311144A (en) * 2018-01-04 2018-07-24 广东药科大学 A kind of dumbbell shaped nanogold-platinum composite catalyst and preparation method thereof
CN108672716A (en) * 2018-05-23 2018-10-19 厦门斯贝克科技有限责任公司 A kind of preparation method of silver gold-covered nano stick
CN108927151A (en) * 2018-06-08 2018-12-04 南京邮电大学 The method for preparing golden platinum core-shell nanostructure material
CN109752371A (en) * 2018-12-28 2019-05-14 南京邮电大学 For Hg2+The colorimetric of detection/SERS bimodulus probe preparation method and application
CN110715966A (en) * 2018-02-06 2020-01-21 红河学院 Gold platinum core-shell nanorod, preparation method thereof and application thereof in preparing AFB (atomic fluorescence Spectroscopy)1Use of electrochemical sensors

Patent Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101450380A (en) * 2007-12-03 2009-06-10 国家纳米科学中心 Bimetal nano rod of branched gold core/platinum shell structure and preparation method thereof
CN101623762A (en) * 2008-07-09 2010-01-13 国家纳米科学中心 Island-shaped porous tri-metal nano rod with gold core/silver-platinum alloy shell structure and method for preparing same
CN101992294A (en) * 2009-08-19 2011-03-30 三星电机株式会社 Method for preparing metal nanoparticles using matal seed and metal nanoparticles comprising metal seed
US20110278497A1 (en) * 2010-05-11 2011-11-17 China Medical University Nanometal dispersion and method for preparing the same
CN106862581A (en) * 2015-12-10 2017-06-20 济南大学 A kind of concave surface gold@silver platinum Heterogeneous Composite nano-particles with superior catalytic and absorbing properties and preparation method thereof
KR101767342B1 (en) * 2016-07-29 2017-08-10 성균관대학교산학협력단 Multi block nanorods and method fabricating thereof
KR20180019888A (en) * 2016-08-17 2018-02-27 한림대학교 산학협력단 Gold multipod nanoparticle core-platinium shell nanoparticles and synthetic method thereof
WO2018069646A1 (en) * 2016-10-13 2018-04-19 Universite Paris Diderot Synthesis of core-shell nanoparticles and uses of said nanoparticles for surface-enhanced raman spectroscopy
CN108311144A (en) * 2018-01-04 2018-07-24 广东药科大学 A kind of dumbbell shaped nanogold-platinum composite catalyst and preparation method thereof
CN108031840A (en) * 2018-01-15 2018-05-15 国家纳米科学中心 A kind of heterogeneous nano-superstructure of self-supporting metal and its preparation method and application
CN110715966A (en) * 2018-02-06 2020-01-21 红河学院 Gold platinum core-shell nanorod, preparation method thereof and application thereof in preparing AFB (atomic fluorescence Spectroscopy)1Use of electrochemical sensors
CN108672716A (en) * 2018-05-23 2018-10-19 厦门斯贝克科技有限责任公司 A kind of preparation method of silver gold-covered nano stick
CN108927151A (en) * 2018-06-08 2018-12-04 南京邮电大学 The method for preparing golden platinum core-shell nanostructure material
CN109752371A (en) * 2018-12-28 2019-05-14 南京邮电大学 For Hg2+The colorimetric of detection/SERS bimodulus probe preparation method and application

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
张艳萍: ""金/银/铂异质结纳米棒的液相合成及其性能研究"", 《中国优秀硕士学位论文全文数据库(工程科技I辑)》 *
张艳萍: ""金/银/铂异质结纳米棒的液相合成及其性能研究"", 《中国优秀硕士学位论文全文数据库(工程科技I辑)》, 15 December 2013 (2013-12-15), pages 20 - 47 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113500199A (en) * 2021-06-10 2021-10-15 浙江大学 Preparation method of gold-platinum-based bimetallic active oxygen self-generating nano material, product and application thereof
CN115998865A (en) * 2022-12-27 2023-04-25 山东大学 Platinum-gold nanorod@MOF composite material and preparation method and application thereof

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