CN101612567A - A kind of preparation method of three-dimensional porous nano-Au catalyst - Google Patents
A kind of preparation method of three-dimensional porous nano-Au catalyst Download PDFInfo
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- CN101612567A CN101612567A CN200910067291A CN200910067291A CN101612567A CN 101612567 A CN101612567 A CN 101612567A CN 200910067291 A CN200910067291 A CN 200910067291A CN 200910067291 A CN200910067291 A CN 200910067291A CN 101612567 A CN101612567 A CN 101612567A
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Abstract
The invention belongs to a kind of preparation method of three-dimensional porous nano-Au catalyst, the present invention is a raw material with copper sulphate, sulfuric acid, Copper Foil, gold chloride, selects H
2Template prepares three-dimensional porous nano-Au catalyst, and the concentration of copper sulphate is 0.125～0.400M, and the concentration of sulfuric acid is 0.500～1.500M; Sand papering, cleaning Copper Foil, is the color of bright metallic copper until its surface; Intercepting 1 * 1cm
2Copper Foil, with mash welder with wire bonds to Copper Foil; With the Copper Foil is negative electrode, and platinized platinum is anode acid copper under 3.0～5.0V voltage, and sedimentation time is 60～120s; It is the 60ml aqueous solution of 1.000～3.000mM that Copper Foil is placed gold chloride concentration, leaves standstill 5～9h under the room temperature, promptly makes three-dimensional porous nano-Au catalyst.Hole is of a size of 20～40 μ m, and golden nanometer particle is of a size of 2～5nm, and the skeleton wall thickness that golden nanometer particle is piled up is 10～20 μ m.Preparation method's technology of the present invention is simple, with low cost, but and continuous batch production.
Description
Technical field
The invention belongs to a kind of preparation method of three-dimensional porous nano-Au catalyst.
Background technology
Fluffy pore space structure helps the exchange of material in the three-dimensional porous nano-Au metal catalyst, and big surface area helps the catalysis of electrochemical reaction, this just makes the three-dimensional porous nano-Au metal catalyst be fit to very much do electrochemical device, such as sensor, the electrode material of fuel cell and battery etc.Therefore, the synthetic and application study of three-dimensional porous nano-Au metal catalyst has caused the great interest of people.At present, mainly be based on H
2Template (Chem.Mater.2004,16:5460-5464) preparation three-dimensional porous nano-Au metal catalyst.But gold can not directly be used H
2Template is synthetic, because gold itself has very high equilibrium potential and lower hydrogen overpotential, this makes the Au surface have only H
2Separate out and do not have the reduction of Au.Cu, Ni, the porous nanometer structure of metals such as Sn can be used H
2Template is synthetic, and therefore, the preparation of porous nano-Au is at H
2Dynamic template form behind the Cu film of loose structure again by displacement reaction obtain (Electrochem.Commu.2007,9:981-988).Its method is: pass through H earlier
2The Cu film that template is synthesizing porous obtains the porous Au film that Cu supports by displacement reaction again between Cu film and Au salt.The H that uses in the method
2Simple, the realization, pollution-free easily of template is with the substrate of Cu as the Au catalyst of supporting three-dimensional porous structure, low price.
Summary of the invention
The purpose of this invention is to provide a kind of three-dimensional porous nano-Au catalyst;
Another object of the present invention provides a kind of preparation method of three-dimensional porous nano-Au catalyst.
For exploring low cost, the method for high-quality and large batch of production three-dimensional porous nano-Au catalyst, the present invention is a raw material with copper sulphate, sulfuric acid, Copper Foil, gold chloride, selects free of contamination H
2Template and low-cost copper are as supporting substrate scale preparation three-dimensional porous nano-Au catalyst.
Three-dimensional porous nano-Au reaction of formation mechanism of the present invention is:
3Cu+2AuCl
4 -＝3Cu
2++2Au+8Cl
-
Realize that preparation process of the present invention is as follows:
1), Copper Foil is handled with sand papering, uses sulfuric acid more respectively, ethanol, deionized water ultrasonic cleaning, drying;
2), treat to be cut into 1 * 1cm after the Copper Foil drying
2Square small pieces, with mash welder with wire bonds to Copper Foil;
3), copper-bath is mixed with sulfuric acid solution, the concentration of copper sulphate is 0.125～0.400M in the mixed liquor, and the concentration of sulfuric acid is 0.500～1.500M;
4), Copper Foil, the platinized platinum electrode of handling well placed above mixed liquor respectively, and to keep distance between the two be 2cm, and platinized platinum, Copper Foil are linked to each other with D.C. regulated power supply anode, negative electrode respectively;
5), connect power supply, controlling two interelectrode voltages is 3.0～5.0V, electric current 0.250～1.220A uses H
2The dynamic template acid copper, the control sedimentation time is 60～120s;
6), the electro-deposition copper foil that obtains is placed the aqueous solution of chloraurate of 1.000～3.000mM, leave standstill 5～9h;
7), Copper Foil is down dry in normal temperature, promptly obtain three-dimensional porous nano-Au catalyst, hole is of a size of 20～40 μ m, golden nanometer particle is of a size of 2～5nm, the skeleton structure that golden nanometer particle is piled up is 10～20 μ m.
X ray electron diffraction analysis according to the prepared three-dimensional porous nano-Au catalyst of said method shows: product is the mixture of copper and gold.Further scanning electron microscope analysis shows: product is a three-dimensional porous nano-Au, and hole is of a size of 20～40 μ m, and golden nanometer particle is of a size of 2～5nm, and the skeleton structure that golden nanometer particle is piled up is 10～20 μ m.
The three-dimensional porous nano-Au catalyst of the present invention's preparation is loose structure and high surface area is arranged, and helps the exchange of material and the raising of catalytic activity, and is the support material of porous with cheap copper, and is with low cost; The preparation method of three-dimensional porous nano-Au catalyst is based on the H2 template, and is pollution-free, and technology is simple, but and continuous batch production.
The specific embodiment
Embodiment 1:
Copper Foil is handled with sand papering, used sulfuric acid then respectively, ethanol, deionized water ultrasonic cleaning, drying.Treat to be cut into 1 * 1cm after the Copper Foil drying
2Square small pieces, again with mash welder with wire bonds to Copper Foil.The copper-bath of 0.250M was mixed with the 1.000M sulfuric acid solution in 1: 1 by volume, and the concentration that makes copper sulphate in the solution is 0.125M, and sulfuric acid concentration is 0.500M.Copper Foil, the platinized platinum electrode handled well are placed mixed liquor respectively, and to keep distance between the two be 2cm, platinized platinum, Copper Foil are linked to each other with D.C. regulated power supply anode, negative electrode respectively.Connect power supply, controlling two interelectrode voltages is 3.0V, and electric current 0.250A uses H
2Dynamic template method acid copper, the control sedimentation time is 120s.The electro-deposition copper foil that obtains is placed the 60ml aqueous solution of chloraurate of 3.000mM, leave standstill 5h.Above sample normal temperature is dry down, promptly obtain three-dimensional porous nano-Au catalyst.Hole is of a size of 23 μ m, and golden nanometer particle is of a size of 5nm, and the skeleton wall thickness that golden nanometer particle is piled up is 19 μ m.
Embodiment 2:
Copper Foil is handled with sand papering, used sulfuric acid then respectively, ethanol, deionized water ultrasonic cleaning, drying.Treat to be cut into 1 * 1cm after the Copper Foil drying
2Square small pieces, with mash welder wire bonds is arrived again
On the Copper Foil.The copper-bath of 0.250M was mixed with the 1.000M sulfuric acid solution in 1: 1 by volume, and the concentration that makes copper sulphate in the solution is 0.125M, and sulfuric acid concentration is 0.500M.Copper Foil, the platinized platinum electrode handled well are placed mixed liquor respectively, and to keep distance between the two be 2cm, platinized platinum, Copper Foil are linked to each other with D.C. regulated power supply anode, negative electrode respectively.Connect power supply, controlling two interelectrode voltages is 4.0V, and electric current 0.620A uses H
2Dynamic template method acid copper, the control sedimentation time is 90s.The electro-deposition copper foil that obtains is placed the 60ml aqueous solution of chloraurate of 2.000mM, leave standstill 7h.Above sample normal temperature is dry down, promptly obtain three-dimensional porous nano-Au catalyst.Hole is of a size of 23 μ m, and golden nanometer particle is of a size of 4nm, and the skeleton wall thickness that golden nanometer particle is piled up is 17 μ m.
Embodiment 3:
Copper Foil is handled with sand papering, used sulfuric acid then respectively, ethanol, deionized water ultrasonic cleaning, drying.Treat to be cut into 1 * 1cm after the Copper Foil drying
2Square small pieces, again with mash welder with wire bonds to Copper Foil.The copper-bath of 0.250M was mixed with the 1.000M sulfuric acid solution in 1: 1 by volume, and the concentration that makes copper sulphate in the solution is 0.125M, and sulfuric acid concentration is 0.500M.Copper Foil, the platinized platinum electrode handled well are placed mixed liquor respectively, and to keep distance between the two be 2cm, platinized platinum, Copper Foil are linked to each other with D.C. regulated power supply anode, negative electrode respectively.Connect power supply, controlling two interelectrode voltages is 5.0V, and electric current 1.220A uses H
2Dynamic template method acid copper, the control sedimentation time is 60s.The electro-deposition copper foil that obtains is placed the 60ml aqueous solution of chloraurate of 1.000mM, leave standstill 9h.Above sample normal temperature is dry down, promptly obtain three-dimensional porous nano-Au catalyst.Hole is of a size of 20 μ m, and golden nanometer particle is of a size of 5nm, and the skeleton wall thickness that golden nanometer particle is piled up is 20 μ m.
Embodiment 4:
Copper Foil is handled with sand papering, used sulfuric acid then respectively, ethanol, deionized water ultrasonic cleaning, drying.Treat to be cut into 1 * 1cm after the Copper Foil drying
2Square small pieces, again with mash welder with wire bonds to Copper Foil.The copper-bath of 0.400M was mixed with the 2.000M sulfuric acid solution in 1: 1 by volume, and the concentration that makes copper sulphate in the solution is 0.200M, and sulfuric acid concentration is 1.000M.Copper Foil, the platinized platinum electrode handled well are placed mixed liquor respectively, and to keep distance between the two be 2cm, platinized platinum, Copper Foil are linked to each other with D.C. regulated power supply anode, negative electrode respectively.Connect power supply, controlling two interelectrode voltages is 3.0V, and electric current 0.250A uses H
2Dynamic template method acid copper, the control sedimentation time is 120s.The electro-deposition copper foil that obtains is placed the 60ml aqueous solution of chloraurate of 3.000mM, leave standstill 5h.Above sample normal temperature is dry down, promptly obtain three-dimensional porous nano-Au catalyst.Hole is of a size of 30 μ m, and golden nanometer particle is of a size of 4nm, and the skeleton wall thickness that golden nanometer particle is piled up is 16 μ m.
Embodiment 5:
Copper Foil is handled with sand papering, used sulfuric acid then respectively, ethanol, deionized water ultrasonic cleaning, drying.Treat to be cut into 1 * 1cm after the Copper Foil drying
2Square small pieces, again with mash welder with wire bonds to Copper Foil.The copper-bath of 0.400M was mixed with the 2.000M sulfuric acid solution in 1: 1 by volume, and the concentration that makes copper sulphate in the solution is 0.200M, and sulfuric acid concentration is 1.000M.Copper Foil, the platinized platinum electrode handled well are placed mixed liquor respectively, and to keep distance between the two be 2cm, platinized platinum, Copper Foil are linked to each other with D.C. regulated power supply anode, negative electrode respectively.Connect power supply, controlling two interelectrode voltages is 4.0V, and electric current 0.620A uses H
2Dynamic template method acid copper, the control sedimentation time is 90s.The electro-deposition copper foil that obtains is placed the 60ml aqueous solution of chloraurate of 2.000mM, leave standstill 7h.Above sample normal temperature is dry down, promptly obtain three-dimensional porous nano-Au catalyst.Hole is of a size of 33 μ m, and golden nanometer particle is of a size of 4nm, and the skeleton wall thickness that golden nanometer particle is piled up is 14 μ m.
Embodiment 6:
Copper Foil is handled with sand papering, used sulfuric acid then respectively, ethanol, deionized water ultrasonic cleaning, drying.Treat to be cut into 1 * 1cm after the Copper Foil drying
2Square small pieces, again with mash welder with wire bonds to Copper Foil.The copper-bath of 0.400M was mixed with the 2.000M sulfuric acid solution in 1: 1 by volume, and the concentration that makes copper sulphate in the solution is 0.200M, and sulfuric acid concentration is 1.000M.Copper Foil, the platinized platinum electrode handled well are placed mixed liquor respectively, and to keep distance between the two be 2cm, platinized platinum, Copper Foil are linked to each other with D.C. regulated power supply anode, negative electrode respectively.Connect power supply, controlling two interelectrode voltages is 5.0V, and electric current 1.220A uses H
2Dynamic template method acid copper, the control sedimentation time is 60s.The electro-deposition copper foil that obtains is placed the 60ml aqueous solution of chloraurate of 1.000mM, leave standstill 9h.Above sample normal temperature is dry down, promptly obtain three-dimensional porous nano-Au catalyst.Hole is of a size of 29 μ m, and golden nanometer particle is of a size of 5nm, and the skeleton wall thickness that golden nanometer particle is piled up is 16 μ m.
Embodiment 7:
Copper Foil is handled with sand papering, used sulfuric acid then respectively, ethanol, deionized water ultrasonic cleaning, drying.Treat to be cut into 1 * 1cm after the Copper Foil drying
2Square small pieces, again with mash welder with wire bonds to Copper Foil.The copper-bath of 0.800M was mixed with the 3.000M sulfuric acid solution in 1: 1 by volume, and the concentration that makes copper sulphate in the solution is 0.400M, and sulfuric acid concentration is 1.500M.Copper Foil, the platinized platinum electrode handled well are placed mixed liquor respectively, and to keep distance between the two be 2cm, platinized platinum, Copper Foil are linked to each other with D.C. regulated power supply anode, negative electrode respectively.Connect power supply, controlling two interelectrode voltages is 3.0V, and electric current 0.250A uses H
2Dynamic template method acid copper, the control sedimentation time is 120s.The electro-deposition copper foil that obtains is placed the 60ml aqueous solution of chloraurate of 3.000mM, leave standstill 5h.Above sample normal temperature is dry down, promptly obtain three-dimensional porous nano-Au catalyst.Hole is of a size of 38 μ m, and golden nanometer particle is of a size of 3nm, and the skeleton wall thickness that golden nanometer particle is piled up is 12 μ m.
Embodiment 8:
Copper Foil is handled with sand papering, used sulfuric acid then respectively, ethanol, deionized water ultrasonic cleaning, drying.Treat to be cut into 1 * 1cm after the Copper Foil drying
2Square small pieces, again with mash welder with wire bonds to Copper Foil.The copper-bath of 0.800M was mixed with the 3.000M sulfuric acid solution in 1: 1 by volume, and the concentration that makes copper sulphate in the solution is 0.400M, and sulfuric acid concentration is 1.500M.Copper Foil, the platinized platinum electrode handled well are placed mixed liquor respectively, and to keep distance between the two be 2cm, platinized platinum, Copper Foil are linked to each other with D.C. regulated power supply anode, negative electrode respectively.Connect power supply, controlling two interelectrode voltages is 4.0V, and electric current 0.620A uses H
2Dynamic template method acid copper, the control sedimentation time is 90s.The electro-deposition copper foil that obtains is placed the 60ml aqueous solution of chloraurate of 2.000mM, leave standstill 7h.Above sample normal temperature is dry down, promptly obtain three-dimensional porous nano-Au catalyst.Hole is of a size of 40 μ m, and golden nanometer particle is of a size of 2nm, and the skeleton wall thickness that golden nanometer particle is piled up is 10 μ m.
Embodiment 9:
Copper Foil is handled with sand papering, used sulfuric acid then respectively, ethanol, deionized water ultrasonic cleaning, drying.Treat to be cut into 1 * 1cm after the Copper Foil drying
2Square small pieces, again with mash welder with wire bonds to Copper Foil.The copper-bath of 0.800M was mixed with the 3.000M sulfuric acid solution in 1: 1 by volume, and the concentration that makes copper sulphate in the solution is 0.400M, and sulfuric acid concentration is 1.500M.Copper Foil, the platinized platinum electrode handled well are placed mixed liquor respectively, and to keep distance between the two be 2cm, platinized platinum, Copper Foil are linked to each other with D.C. regulated power supply anode, negative electrode respectively.Connect power supply, controlling two interelectrode voltages is 5.0V, and electric current 1.220A uses H
2Dynamic template method acid copper, the control sedimentation time is 60s.The electro-deposition copper foil that obtains is placed the 60ml aqueous solution of chloraurate of 1.000mM, leave standstill 9h.Above sample normal temperature is dry down, promptly obtain three-dimensional porous nano-Au catalyst.Hole is of a size of 38 μ m, gold
Nano particle is of a size of 4nm, and the skeleton wall thickness that golden nanometer particle is piled up is 13 μ m.
Claims (2)
1, a kind of three-dimensional porous nano-Au catalyst, hole are of a size of 20～40 μ m, and golden nanometer particle is of a size of 2～5nm, and the skeleton wall thickness that golden nanometer particle is piled up is 10～20 μ m;
2, a kind of preparation method of three-dimensional porous nano-Au catalyst is characterized in that preparation process is as follows:
1), Copper Foil is handled with sand papering, uses sulfuric acid more respectively, ethanol, deionized water ultrasonic cleaning, drying;
2), treat to be cut into 1 * 1cm after the Copper Foil drying
2Square small pieces, with mash welder with wire bonds to Copper Foil;
3), copper-bath is mixed with sulfuric acid solution, the concentration of copper sulphate is 0.125～0.400M in the mixed liquor, and the concentration of sulfuric acid is 0.500～1.500M;
4), Copper Foil, the platinized platinum electrode of handling well placed above mixed liquor respectively, and to keep distance between the two be 2cm, and platinized platinum, Copper Foil are linked to each other with D.C. regulated power supply anode, negative electrode respectively;
5), connect power supply, controlling two interelectrode voltages is 3.0～5.0V, electric current 0.250～1.220A uses H
2The dynamic template acid copper, the control sedimentation time is 60～120s;
6), the electro-deposition copper foil that obtains is placed the aqueous solution of chloraurate of 1.000～3.000mM, leave standstill 5～9h;
7), Copper Foil is down dry in normal temperature, promptly obtain three-dimensional porous nano-Au catalyst, hole is of a size of 20～40 μ m, golden nanometer particle is of a size of 2～5nm, the skeleton structure that golden nanometer particle is piled up is 10～20 μ m.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103331171A (en) * | 2013-07-08 | 2013-10-02 | 华东理工大学 | Preparation method and applications of catalyst used for preparing light olefin from synthesis gas |
| CN112151817A (en) * | 2020-10-26 | 2020-12-29 | 中北大学 | Copper-based anode catalyst for direct methanol fuel cell and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101433959A (en) * | 2008-12-22 | 2009-05-20 | 中国科学院长春应用化学研究所 | Method for preparing hollow nano gold powder material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103331171A (en) * | 2013-07-08 | 2013-10-02 | 华东理工大学 | Preparation method and applications of catalyst used for preparing light olefin from synthesis gas |
| CN103331171B (en) * | 2013-07-08 | 2015-02-18 | 华东理工大学 | Preparation method and applications of catalyst used for preparing light olefin from synthesis gas |
| CN112151817A (en) * | 2020-10-26 | 2020-12-29 | 中北大学 | Copper-based anode catalyst for direct methanol fuel cell and preparation method thereof |
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