CN102581273A - Porous core-shell nano auriferous alloy and preparation method for same - Google Patents
Porous core-shell nano auriferous alloy and preparation method for same Download PDFInfo
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- CN102581273A CN102581273A CN2012100544834A CN201210054483A CN102581273A CN 102581273 A CN102581273 A CN 102581273A CN 2012100544834 A CN2012100544834 A CN 2012100544834A CN 201210054483 A CN201210054483 A CN 201210054483A CN 102581273 A CN102581273 A CN 102581273A
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Abstract
The invention discloses a porous core-shell nano auriferous alloy and a preparation method for the same. The alloy comprises an Au (gold) core and a metal shell of a porous structure, the thickness of the shell ranges from 25nm to 35nm, and components of the shell consist of Au, Pd (palladium), Pt (platinum) and alloy of Au, Pd and Pt. Compared with the prior art, the method is used for preparing a porous core-shell auriferous alloy nano structure by using low-valence (univalent or divalent) noble metal saline solution as raw materials. The method is simple, controllable, high in reproducibility and generally applicable, and purity approximates 100%. Compared with a monocrystal core-shell nano structure, the porous core-shell auriferous alloy nano structure is larger in specific surface area and more excellent in catalysis, and can be used for heterogeneous catalysis and used as electrode materials for electro-catalysis and fuel cells.
Description
Technical field:
The invention belongs to this technical field of inorganic nano material and preparation method thereof.
Technical background:
Two during the last ten years, and the function nano material has shown surprising using value and potential quality at the key areas that energy catalysis, organic catalysis, photocatalysis etc. concern lifelines of the national economy.Especially noble metal nano structure (for example Au, Pd and Pt etc.) is extensively paid close attention to because of having excellent catalytic performance.The catalytic performance of the big bright nano catalytic material of quantity research fact table has significant structure dependence, and therefore studying and construct the high-activity nano structure is to solve one of catalysis key of problem.In recent years, the core-shell nano structure obtains extensive concern, has the catalytic activity and the catalytic stability of remarkable enhancing in fields such as lithium ion battery, energy catalysis, organic catalysis.This structure is to be made up of nuclear and shell, and the component of nucleocapsid can be regulated as required, brings some novel character and catalysis behavior when possessing nuclear and shell component material dual-use function again.In addition, because the metal polycrystalline Nano structure of porous has bigger specific area, more catalytic activity position is so have catalytic activity and the stability more superior than monocrystal nanostructure.Yet the metal shell that obtains the metal core shell structure at present is a mono-crystalline structures, so catalytic activity is still limited.
Summary of the invention:
The present invention is directed to the limited problem of monocrystalline nucleocapsid metal Nano structure catalytic activity, a kind of porous Au-M (M=Au, Pd, Pt and alloy thereof) core-shell nano structure catalyst and preparation method thereof is provided.
A kind of porous Au-M of the present invention (M=Au, Pd, Pt and alloy thereof) core-shell nano structure catalyst is made up of Au nuclear and metal-back, and shell is a loose structure, thickness 25-35nm, and the shell component can be metal and alloys thereof such as Au, Pd.
Technical matters of the present invention comprises the following steps:
A, preparation AuAg core-shell nano: according to existing reported method synthetic (M.Tsuji etc., Cryst.Growth Des.2006,6,1801).Be about to AgNO
3, polyvinylpyrrolidone and Au nano particle join in the ethylene glycol successively, 140 ℃ of reactions 2 hours, water and absolute ethyl alcohol wash 2-3 time successively;
B, ready reaction solution: the configuration lower valency precious metal salt aqueous solution under the room temperature;
In order to obtain HAuCl
2Solution joins HAuCl with 2mL concentration for the 1mmol ascorbic acid solution
4Solution stirring at room 3-5 minute;
C, preparation section: the AuAg core-shell nano is dispersed in the deionized water, adds the lower valency precious metal salt solution, left standstill under the dark condition 2-6 hour, temperature is between 20-80 ℃; The mol ratio of AuAg core-shell nano and lower valency precious metal salt solution is 1: (1.5-0.5);
D, washing: product is centrifugal, and collecting precipitation washs 1-3 time with ammoniacal liquor, deionized water and absolute ethyl alcohol successively, promptly gets porous Au-M (M=Au, Pd, Pt and alloy thereof) core-shell nano structure, and shell is made up of metal nanoparticle, thickness 25-35 nanometer.
Described lower valency is 1, divalent;
Described lower valency precious metal salt solution is: HAuCl
2, H
2PdCl
4, K
2PtCl
4And mixed solution.
When nucleocapsid structure is Au-Au, Au-Pd, when Au-Au/Pd and Au-Au/Pt, preferred reaction temperature is a room temperature;
When nucleocapsid structure was Au-Pt and Au-Pt/Pd, preferred reaction temperature was 60 ℃.
Reaction principle is (is example with Au-Pd):
AuAg+H
2PdCl
4→Au-Pd/AgCl (1)
Au-Pd/AgCl+NH
3·H
2O→Au-Pd+Ag(NH
3)
2 + (2)
The advantage that the present invention gives prominence to is: adopting lower valency (monovalence or divalence) precious metal salt solution is raw material, prepares a kind of porous nucleocapsid gold alloy nanostructured nanostructured.The method simple controllable, purity is nearly 100%, and repeatability is strong, and can generally be suitable for.Compare with monocrystalline core-shell nano structure, this porous nucleocapsid gold alloy nanostructured has bigger specific area, has excellent more catalytic performance, the electrode material that can be used for heterogeneous catalysis and be used as electro-catalysis and fuel cell.
Description of drawings:
Fig. 1 is the TEM photo of the porous Au-Au core-shell nano structure catalyst that makes of embodiment 1.
Fig. 2 is the TEM photo of the porous Au-Pd core-shell nano structure catalyst that makes of embodiment 2.
Fig. 3 is the TEM photo of the porous Au-Pt core-shell nano structure catalyst that makes of embodiment 3.
Fig. 4 is the cyclic voltammetry curve of the porous Au-Pd core-shell nano structure catalyst electro-catalysis oxidation of ethanol that makes of embodiment 2.
Fig. 5 is the linear scan volt-ampere curve of the porous Au-Pd core-shell nano structure catalyst electro-catalysis oxygen reduction that makes of embodiment 2.
The specific embodiment:
Be the non-limiting preparation embodiment of the present invention below, the present invention further described through these embodiment.
Embodiment 1:
Take by weighing 1.2mg AuAg core-shell nano, be dispersed in the 10mL deionized water, adding 1mL concentration is the HAuCl of 10.2mmol/L
2Left standstill under the solution, dark condition 2 hours, temperature is a room temperature.Product is centrifugal, and collecting precipitation washs with ammoniacal liquor, deionized water and absolute ethyl alcohol successively, promptly makes porous Au-Au core-shell nano structure, and as shown in Figure 1, shell is made up of the Au nano particle, about 35 nanometers of thickness.
Embodiment 2:
Take by weighing 2.4mg AuAg core-shell nano, be dispersed in the 15mL deionized water, adding 2mL concentration is the H of 13.5mmol/L
2PdCl
4Left standstill under the aqueous solution, dark condition 4 hours, temperature is a room temperature.Product is centrifugal, and collecting precipitation washs with ammoniacal liquor, deionized water and absolute ethyl alcohol successively, promptly makes porous Au-Pd core-shell nano structure, and as shown in Figure 2, shell is made up of the Pd nano particle, about 25 nanometers of thickness.
Embodiment 3:
Take by weighing 1.5mg AuAg core-shell nano, be dispersed in the 12mL deionized water, adding 1.5mL concentration is the K of 18.5mmol/L
2PtCl
4Left standstill under the aqueous solution, dark condition 6 hours, temperature is 60 ℃.Product is centrifugal, and collecting precipitation washs with ammoniacal liquor, deionized water and absolute ethyl alcohol successively, promptly makes porous Au-Pt core-shell nano structure, and as shown in Figure 3, shell is made up of the Pt nano particle, about 30 nanometers of thickness.
Embodiment 4:
Take by weighing 2mg AuAg core-shell nano, be dispersed in the 15mL deionized water, adding 1.5mL concentration is the H of 13.5mmol/L
2PdCl
4Left standstill under the aqueous solution, dark condition 4 hours, temperature is 40 ℃.Product is centrifugal, and collecting precipitation washs with ammoniacal liquor, deionized water and absolute ethyl alcohol successively, promptly makes porous Au-Pd core-shell nano structure, and shell is made up of the Pd nano particle, about 25 nanometers of thickness.
Embodiment 5:
Take by weighing 2.4mg AuAg core-shell nano, be dispersed in the 15mL deionized water, adding 2mL concentration is the H of 13.5mmol/L
2PdCl
4Left standstill under the aqueous solution, dark condition 2 hours, temperature is 45 ℃.Product is centrifugal, and collecting precipitation washs with ammoniacal liquor, deionized water and absolute ethyl alcohol successively, promptly makes porous Au-Pd core-shell nano structure, and shell is made up of the Pd nano particle, about 25 nanometers of thickness.
Embodiment 6:
Take by weighing 1.2mg AuAg core-shell nano, be dispersed in the 12mL deionized water, adding 1.5mL concentration is the HAuCl of 10.2mmol/L
2The H of solution and 13.5mmol
2PdCl
4Left standstill under the mixed solution, dark condition 2 hours, temperature is a room temperature.Product is centrifugal, and collecting precipitation washs with ammoniacal liquor, deionized water and absolute ethyl alcohol successively, promptly makes porous Au-Au/Pd core-shell nano structure, and shell is made up of the Au/Pd alloy nanoparticle, about 30 nanometers of thickness.
Embodiment 7:
Take by weighing 1.2mg AuAg core-shell nano, be dispersed in the 12mL deionized water, adding 1.5mL concentration is the K of 18.5mmol/L
2PtCl
4The H of solution and 13.5mmol
2PdCl
4Left standstill under the mixed solution, dark condition 3 hours, temperature is 50 ℃.Product is centrifugal, and collecting precipitation washs with ammoniacal liquor, deionized water and absolute ethyl alcohol successively, promptly makes porous Au-Pt/Pd core-shell nano structure, and shell is made up of the Pt/Pd alloy nanoparticle, about 30 nanometers of thickness.
Embodiment 8:
Take by weighing 2.1mg AuAg core-shell nano, be dispersed in the 10mL deionized water, adding 1.5mL concentration is the K of 18.5mmol/L
2PtCl
4The HAuCl of solution and 10.2mmol
2Mixed solution, left standstill under the dark condition 5 hours, temperature is 60 ℃.Product is centrifugal, and collecting precipitation washs with ammoniacal liquor, deionized water and absolute ethyl alcohol successively, promptly makes porous Au-Pt/Au core-shell nano structure, and shell is made up of the Pt/Au alloy nanoparticle, about 25 nanometers of thickness.
Embodiment 9:
The evaluation method of a kind of porous core-shell nano gold alloy catalytic performance of the present invention (is example with the Au-Pd electro-catalysis):
The glass-carbon electrode of 3mm diameter is used 0.3 and 0.05 μ m γ-Al successively
2O
3The powder polishing.With the ultrasonic 1mL absolute ethyl alcohol that is scattered in of 1mg porous Au-Pd nuclear shell structure nano catalyst.Drip the above-mentioned ethanolic solution of 20 μ L then on the glass-carbon electrode after the polishing.After the drying, drip 10 μ L Nafion (0.05wt%) solution on above-mentioned electrode, air dry gets final product.Like this, modifying (work) electrode has just prepared.Electrochemical measurement carries out on the work station of three-electrode system.Wherein, the conduct of Pt silk electrode is to electrode, and modified electrode is as working electrode.All are measured all at room temperature.
(1) electro-catalysis oxidation of ethanol: in 0.5mol/L KOH and 0.5mol/L ethanolic solution, carry out, sweep speed and be 50mV/s, Ag/AgCl (KCl is saturated) electrode is as reference electrode.
As shown in Figure 5: porous Au-Pd nucleocapsid structure is all more superior than the catalytic performance of Pd nano particle and Pt/C catalyst, has better CO-endurance, and the overtrick potential drop of oxidation of ethanol is low.
(2) electro-catalysis oxygen reduction: in the saturated KOH solution of 0.5mol/L oxygen, carry out, sweep speed and be 10mV/s, saturated calomel electrode is as reference electrode.
As shown in Figure 4: porous Au-Pd nucleocapsid structure has more superior catalytic performance than Pd nano particle, increased activity, and the overvoltage of oxygen reduction reduces.
Claims (7)
1. porous core-shell nano gold alloy is characterized in that: described alloy is made up of Au nuclear and metal-back, and shell is a loose structure, thickness 25-35nm, and the shell component is Au, Pd, Pt and alloy thereof.
2. the preparation method of the described a kind of porous core-shell nano gold alloy of claim 1 comprises following operation:
A, preparation AuAg core-shell nano:
B, ready reaction solution: the configuration lower valency precious metal salt aqueous solution under the room temperature;
C, preparation section: the AuAg core-shell nano is dispersed in the deionized water, adds the lower valency precious metal salt solution, left standstill under the dark condition 2-6 hour, temperature is between 20-80 ℃; The mol ratio of AuAg core-shell nano and lower valency precious metal salt solution is 1: (1.5-0.5);
D, washing: product is centrifugal, and collecting precipitation washs 1-3 time with ammoniacal liquor, deionized water and absolute ethyl alcohol successively, gets final product.
3. the preparation method of a kind of porous core-shell nano gold alloy according to claim 2,, it is characterized in that:
Described A, preparation AuAg core-shell nano:
With AgNO
3, polyvinylpyrrolidone and Au nano particle join in the ethylene glycol successively, 140 ℃ of reactions 2 hours, water and absolute ethyl alcohol wash 2-3 time successively; Get final product.
4. the preparation method of a kind of porous core-shell nano gold alloy according to claim 2 is characterized in that:
Described lower valency is 1, divalent.
5. the preparation method of a kind of porous core-shell nano gold alloy according to claim 2 is characterized in that:
Described lower valency precious metal salt solution is: HAuCl
2, H
2PdCl
4, K
2PtCl
4And mixed solution.
6. the preparation method of a kind of porous core-shell nano gold alloy according to claim 2 is characterized in that:
When nucleocapsid structure is Au-Au, Au-Pd, when Au-Au/Pd and Au-Au/Pt, reaction temperature is a room temperature.
7. the preparation method of a kind of porous core-shell nano gold alloy according to claim 2 is characterized in that:
When nucleocapsid structure was Au-Pt and Au-Pt/Pd, reaction temperature was 60 ℃.
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| CN103240422A (en) * | 2013-04-16 | 2013-08-14 | 同济大学 | Method for preparing composite heterostructure of zinc oxide nano rods and silver micron plate |
| CN103600090A (en) * | 2013-12-10 | 2014-02-26 | 天津商业大学 | Au@AuPt alloy nanoparticles and preparation method of colloidal dispersion system |
| CN105817642A (en) * | 2016-04-19 | 2016-08-03 | 南京农业大学 | Au/Ag core shell nanomaterial with efficient antibacterial property and preparation method of Au/Ag core shell nanomaterial |
| CN105880586A (en) * | 2016-04-19 | 2016-08-24 | 南京农业大学 | Au/Ag/Au core-shell nano anti-bacterial material and preparation method thereof |
| CN107309422A (en) * | 2017-05-18 | 2017-11-03 | 中国科学院合肥物质科学研究院 | A kind of porous electrum nano material and preparation method and application |
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| CN103600090B (en) * | 2013-12-10 | 2015-08-19 | 天津商业大学 | The preparation method of Au@AuPt alloy nano particle and colloidal dispersion system |
| CN105817642B (en) * | 2016-04-19 | 2018-04-13 | 南京农业大学 | A kind of Au/Ag core-shell nano materials with Efficient antibacterial performance and preparation method thereof |
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| CN105880586A (en) * | 2016-04-19 | 2016-08-24 | 南京农业大学 | Au/Ag/Au core-shell nano anti-bacterial material and preparation method thereof |
| CN105880586B (en) * | 2016-04-19 | 2017-12-19 | 南京农业大学 | A kind of Au/Ag/Au core-shell nanos antibacterial material and preparation method thereof |
| CN107309422B (en) * | 2017-05-18 | 2019-05-31 | 中国科学院合肥物质科学研究院 | A kind of porous gold-silver alloy nano material and the preparation method and application thereof |
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| CN108273563A (en) * | 2018-02-02 | 2018-07-13 | 江西省科学院应用化学研究所 | A kind of embedded precious metals pd/BiVO4@RuIIIThe preparation method of-TA nuclear-shell structured nano-composite materials |
| CN108421508A (en) * | 2018-02-28 | 2018-08-21 | 五行科技股份有限公司 | A kind of preparation method of the platinum comprising multinuclear-polymer nanocomposite core-shell material |
| CN108421508B (en) * | 2018-02-28 | 2020-05-12 | 五行科技股份有限公司 | Preparation method of multinuclear platinum-polymer nano core-shell material |
| CN113059175A (en) * | 2021-01-08 | 2021-07-02 | 中国石油大学(华东) | Preparation method of Au @ Ag @ AgCl nanoparticles and application of Au @ Ag @ AgCl nanoparticles in ammonia colorimetric detection |
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Application publication date: 20120718 |