CN103817319A - Copper-bearing bimetallic nanometer material with dentritic structure and method for manufacturing copper-bearing bimetallic nanometer material - Google Patents
Copper-bearing bimetallic nanometer material with dentritic structure and method for manufacturing copper-bearing bimetallic nanometer material Download PDFInfo
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- CN103817319A CN103817319A CN201210469962.2A CN201210469962A CN103817319A CN 103817319 A CN103817319 A CN 103817319A CN 201210469962 A CN201210469962 A CN 201210469962A CN 103817319 A CN103817319 A CN 103817319A
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Abstract
The invention discloses a copper-bearing bimetallic nanometer material with a dentritic structure and a method for manufacturing the copper-bearing bimetallic nanometer material. The method includes manufacturing procedures of adding surfactants and mixed solution containing copper and another metal precursor into water solution; adding moderate reducing agents into the water solution to reduce the water solution. The copper-bearing bimetallic nanometer material and the method have the advantages that the dentritic nanometer structure is single in morphology and uniform in size, and components of the copper-bearing bimetallic nanometer material are controllable; raw materials required in the method are cheap and are easily available, the preparation procedures are simple and convenient, elapsed reaction time is short, and safe operation can be implemented; the dentritic nanometer structure can have important application in the catalysis and electrochemistry fields.
Description
Technical field
The present invention relates to a kind of cupric bimetal nano material with dendritic structure and preparation method thereof.
Background technology
The features such as porous, specific area are large owing to having for the metal nano material with dendritic structure, rough surface and the high miller index surface that may exist, there is many application in fields such as catalysis, electrochemistry, optics, therefore there is the metal nano material of dendritic structure and preparation thereof and application and be subject to researcher's extensive concern.
Be monometallic structure about the report majority of dendritic metal nano material at present, and relatively less for the report of dendritic bimetal nanostructure.Crystal seed method is to prepare one of the most frequently used method of dendroid bimetal nanostructure.For example, Eichhorn group is take golden nanometer particle as crystal seed, reduces acetylacetone,2,4-pentanedione platinum in organic solvent oleyl amine/decahydronaphthalene mixed system, successfully made dendroid Au-Pt nanostructured.Xia Younan seminar has also reported a kind of simple water route of synthesis subsequently, take palladium nano-crystal as nucleus, reduce the synthetic three-dimensional Pd-Pt dendroid pattern of potassium chloroplatinate by ascorbic acid, although the method can accurately be controlled pattern and the composition of bimetal nano crystalline substance, but it also has some limitations, as needed high temperature in building-up process, and building-up process need carry out step by step, more complicated.In addition; Yamauchi seminar has reported the method for one-step synthesis dendroid bimetal nanostructure; it is mainly the presoma that simultaneously adds Au, two kinds of metals of Pt in the protectant aqueous solution of F127 to containing; then reduce by ascorbic acid; obtain having the Au@Pt dendroid bimetal nano crystalline substance of nucleocapsid structure; adopt similar procedure can also synthesize three component Au@Pd@Pt and Pt-on-Pd dendritic structures; although the method one step completes; simple to operation; not consuming time, but the method is only applicable to the bimetallic system of platiniferous at present.Thereby, find a kind of bimetallic dendritic structure simple, economic, the synthetic multiple composition of chemical process with universality and remain a very difficult task.
Summary of the invention
One of object of the present invention is to provide a kind of cupric bimetal nano material with dendritic structure.This dendroid bimetal nano material pattern, size evenly, are alloy structure, have larger specific area, will gather around and have broad application prospects in the field such as electrochemistry and catalysis.
Two of object of the present invention is to provide a kind of method of preparing the cupric bimetal nano material with dendritic structure.The method raw material is cheap and easy to get, and preparation process is simple and convenient, and reaction time consumption is few, handling safety, and can synthesize the bimetallic dendroid nano material with multiple composition.
For achieving the above object, technical scheme of the present invention is:
The cupric bimetal nano material with dendritic structure provided by the invention is to assemble growth by metal nanoparticle to form dendroid, and its pattern is single, and size evenly, is alloy structure, has larger specific area.The bimetallic that the component of described dendroid nanostructured is cupric, the molar ratio of copper and another kind of metal is adjustable between 0.001-3, and wherein another metal component is noble metal Au, Ag, Pt or Pd.
The preparation method of the cupric bimetal nano material with dendritic structure provided by the invention, its preparation process is:
(1) surfactant is joined in the aqueous solution, stir it is dissolved, wherein the concentration of surfactant is 0.1-10mM;
(2) to the presoma that adds copper presoma and another metal in this mixed solution, stirring makes it form the reaction system solution of homogeneous, wherein in reaction system, the concentration of copper ion is 7.5-100mM, and the concentration of another metal ion is 0.1-10mM;
(3) in above-mentioned solution system, add reducing agent reduction, wherein reducing agent adds with the form of the aqueous solution, and the concentration of aqueous solution of reducing agent is 0.01-1M; Reducing agent consumption is 1-20 times of two kinds of metal component total mole numbers.
(4) reacted solution is carried out to centrifugation, the washing of solid nano material, obtain dendritic nano material.
Surfactant used is nonionic surface active agent P123, F127, PVP, PVA, Triton X-100, Brij, Tergitol or Type15-s-7.
The mantoquita that described copper presoma is solubility, comprises one or two or more kinds in the complex of copper nitrate, copper chloride, copper sulphate, Schweinfurt green or copper.
Another described metal precursor is the corresponding chloride of this metal, nitrate, sulfate or acetate.
Reducing agent used is weak reductant, comprises ascorbic acid, formic acid, hydroxylamine hydrochloride, aldehyde compound or inferior sodium phosphate.
The dendritic nano material obtaining is distributed in water stand-by.
The invention has the advantages that:
1, the dendroid cupric bimetal nano material that prepared by the present invention comprises noble metal and two kinds of components of base metal copper, copper add the availability that can improve noble metal, and the content of two kinds of components is adjustable.
2, the dendroid cupric bimetal nano material that prepared by the present invention belongs to the structure of alloy.
3, preparation method's raw material of the present invention is cheap and easy to get, and preparation process is simple and convenient, and reaction time consumption is few, handling safety, and can synthesize the bimetallic dendroid nano material with multiple composition.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of the embodiment of the present invention 1, and XRD and EDS analyze;
Fig. 2 is the transmission electron microscope picture of the embodiment of the present invention 2;
Fig. 3 is the transmission electron microscope picture of the embodiment of the present invention 3;
Fig. 4 is the transmission electron microscope picture of the embodiment of the present invention 4;
Fig. 5 is the transmission electron microscope picture of the embodiment of the present invention 5;
Fig. 6 is the transmission electron microscope picture of the embodiment of the present invention 6;
Fig. 7 is the transmission electron microscope picture of the embodiment of the present invention 7;
Fig. 8 is the transmission electron microscope picture of the embodiment of the present invention 8;
Fig. 9 is the transmission electron microscope picture of the embodiment of the present invention 9;
Figure 10 is the transmission electron microscope picture of the embodiment of the present invention 10;
Figure 11 is the transmission electron microscope picture of the embodiment of the present invention 11;
Figure 12 is the transmission electron microscope picture of the embodiment of the present invention 12;
Figure 13 is the transmission electron microscope picture of the embodiment of the present invention 13.
The specific embodiment
Embodiment 1
Take 50.6mg P123 and join in 20mL sample bottle, add 3.9mL water, stir and make its dissolving; Then add successively 0.875mL, 0.1mol/L Cu (NO
3)
2solution and 0.26mL, 9.56mg
au/ mL HAuCl
4solution, stirs and makes it form the reaction system solution of homogeneous; Add 5mL, 0.1mol/L ascorbic acid reduction 1h; Reacted solution is transferred in centrifuge tube, centrifugation, after washing three times, obtain dendritic golden copper nanostructured, as shown in Figure 1, nano particle is gathered into dendritic nanostructured, and this dendritic nanostructured pattern is single, and size evenly, be of a size of 25nm left and right, know for alloy structure from XRD and EDS analysis.
Embodiment 2
Take 50.6mg P123 and join in 20mL sample bottle, add 2.3mL water, stir and make its dissolving; Then add successively 2.5mL, 0.1mol/L Cu (NO
3)
2solution and 0.26mL, 9.56mg
au/ mL HAuCl
4solution, stirs and makes it form the reaction system solution of homogeneous; Add 5mL, 0.1mol/L ascorbic acid reduction 1h; Reacted solution is transferred in centrifuge tube, and centrifugation, obtains dendritic golden copper nanostructured after washing three times, and as shown in Figure 2, this dendritic nanostructured pattern is single, and mean size is 20nm.
Embodiment 3
Take 50.6mg P123 and join in 20mL sample bottle, add 3.9mL water, stir and make its dissolving; Then add successively 0.875mL, 0.1mol/L CuCl
2solution and 0.26mL, 9.56mg
au/ mLHAuCl
4solution, stirs and makes it form the reaction system solution of homogeneous; Add 5mL, 0.1mol/L ascorbic acid reduction 1h; Reacted solution is transferred in centrifuge tube, and centrifugation, obtains dendritic golden copper nanostructured after washing three times, and as shown in Figure 3, this dendritic nanostructured pattern is single, and mean size is 35nm.
Embodiment 4
Take 50.6mg P123 and join in 20mL sample bottle, add 3.9mL water, stir and make its dissolving; Then add successively 0.875mL, 0.1mol/L CuSO
4solution and 0.26mL, 9.56mg
au/ mL HAuCl
4solution, stirs and makes it form the reaction system solution of homogeneous; Add 5mL, 0.1mol/L ascorbic acid reduction 1h; Reacted solution is transferred in centrifuge tube, and centrifugation, obtains dendritic golden copper nanostructured after washing three times, and as shown in Figure 4, this dendritic nanostructured pattern is single, and mean size is 25nm.
Take 50.6mg F127 and join in 20mL sample bottle, add 3.9mL water, stir and make its dissolving; Then add successively 0.875mL, 0.1mol/L Cu (NO
3)
2solution and 0.26mL, 9.56mg
au/ mL HAuCl
4solution, stirs and makes it form the reaction system solution of homogeneous; Add 5mL, 0.1mol/L ascorbic acid reduction 1h; Reacted solution is transferred in centrifuge tube, and centrifugation, obtains dendritic golden copper nanostructured after washing three times, and as shown in Figure 5, this dendritic nanostructured pattern is single, and mean size is 25nm.
Embodiment 6
Take 50.6mg PVP and join in 20mL sample bottle, add 3.9mL water, stir and make its dissolving; Then add successively 0.875mL, 0.1mol/L Cu (NO
3)
2solution and 0.26mL, 9.56mg
au/ mL HAuCl
4solution, stirs and makes it form the reaction system solution of homogeneous; Add 5mL, 0.1mol/L ascorbic acid reduction 1h; Reacted solution is transferred in centrifuge tube, and centrifugation, obtains dendritic golden copper nanostructured after washing three times, and as shown in Figure 6, this dendritic nanostructured pattern is single, and mean size is 30nm left and right.
Embodiment 7
Take 50.6mg Triton X-100 and join in 20mL sample bottle, add 3.9mL water, stir and make its dissolving; Then add successively 0.875mL, 0.1mol/L Cu (NO
3)
2solution and 0.26mL, 9.56mg
au/ mL HAuCl
4solution, stirs and makes it form the reaction system solution of homogeneous; Add 5mL, 0.1mol/L ascorbic acid reduction 1h; Reacted solution is transferred in centrifuge tube, and centrifugation, obtains dendritic golden copper nanostructured after washing three times, and as shown in Figure 7, this dendritic nanostructured pattern is single, and mean size is 30nm left and right.
Embodiment 8
Take 17.4mg P123 and join in 20mL sample bottle, add 3.9mL water, stir and make its dissolving; Then add successively 0.875mL, 0.1mol/L Cu (NO
3)
2solution and 0.26mL, 9.56mg
au/ mL HAuCl
4solution, stirs and makes it form the reaction system solution of homogeneous; Add 5mL, 0.1mol/L ascorbic acid reduction 1h; Reacted solution is transferred in centrifuge tube, and centrifugation, obtains dendritic golden copper nanostructured after washing three times, and as shown in Figure 8, this dendritic nanostructured pattern is single, and mean size is 30nm left and right.
Embodiment 9
Take 232.1mg P123 and join in 20mL sample bottle, add 3.9mL water, stir and make its dissolving; Then add successively 0.875mL, 0.1mol/L Cu (NO
3)
2solution and 0.26mL, 9.56mg
au/ mL HAuCl
4solution, stirs and makes it form the reaction system solution of homogeneous; Add 5mL, 0.1mol/L ascorbic acid reduction 1h; Reacted solution is transferred in centrifuge tube, and centrifugation, obtains dendritic golden copper nanostructured after washing three times, and as shown in Figure 9, this dendritic nanostructured pattern is single, and mean size is 20nm left and right.
Take 50.6mg P123 and join in 20mL sample bottle, add 4mL water, stir and make its dissolving; Then add successively 0.875mL, 0.1mol/L Cu (NO
3)
2solution and 0.13mL, 9.56mg
au/ mL HAuCl
4solution, stirs and makes it form the reaction system solution of homogeneous; Add 5mL, 0.1mol/L ascorbic acid reduction 1h; Reacted solution is transferred in centrifuge tube, and centrifugation, obtains dendritic golden copper nanostructured after washing three times, and as shown in figure 10, this dendritic nanostructured pattern is single, and mean size is 30nm left and right.
Embodiment 11
Take 50.6mg P123 and join in 20mL sample bottle, add 3.9mL water, stir and make its dissolving; Then add successively 0.875mL, 0.1mol/L Cu (NO
3)
2solution and 0.26mL, 9.56mg
au/ mL HAuCl
4solution, stirs and makes it form the reaction system solution of homogeneous; Add 5mL, 0.05mol/L ascorbic acid reduction 1h; Reacted solution is transferred in centrifuge tube, and centrifugation, obtains dendritic golden copper nanostructured after washing three times, and as shown in figure 11, this dendritic nanostructured pattern is single, and mean size is 30nm left and right.
Embodiment 12
Take 50.6mg P123 and join in 20mL sample bottle, add 4mL water, stir and make its dissolving; Then add successively 0.875mL, 0.1mol/L Cu (NO
3)
2solution and 0.16mL, 14.8mg
pt/ mL H
2ptCl
6solution, stirs and makes it form the reaction system solution of homogeneous; Add 5mL, 0.1mol/L ascorbic acid reduction 1h; Reacted solution is transferred in centrifuge tube, and centrifugation, obtains dendritic golden copper nanostructured after washing three times, and as shown in figure 12, this dendritic nanostructured pattern is single, and mean size is 25nm left and right.
Embodiment 13
Take 50.6mg P123 and join in 20mL sample bottle, add 4mL water, stir and make its dissolving; Then add successively 0.875mL, 0.1mol/L Cu (NO
3)
2solution and 0.11mL, 12.0mg
pd/ mL PdCl
2solution, stirs and makes it form the reaction system solution of homogeneous; Add 5mL, 0.1mol/L ascorbic acid reduction 1h; Reacted solution is transferred in centrifuge tube, and centrifugation, obtains dendritic golden copper nanostructured after washing three times, and as shown in figure 13, this dendritic nanostructured pattern is single, and mean size is 30nm left and right.
Claims (8)
1. a cupric bimetal nano material with dendritic structure, is characterized in that: this dendritic nano material is to assemble growth by metal nanoparticle to form dendroid, and its pattern is single, and size evenly, is alloy structure, has larger specific area.
2. dendroid nanostructured as claimed in claim 1, it is characterized in that: the bimetallic that the component of described dendroid nanostructured is cupric, the molar ratio of copper and another kind of metal is adjustable between 0.001-3, and wherein another metal component is noble metal Au, Ag, Pt or Pd.
3. a preparation method for the cupric bimetal nano material with dendritic structure claimed in claim 1, its preparation process is as follows:
(1) surfactant is joined in the aqueous solution, stir it is dissolved, wherein the concentration of surfactant is 0.1-10mM;
(2) to the presoma that adds copper presoma and another metal in this mixed solution, stirring makes it form the reaction system solution of homogeneous, wherein in reaction system, the concentration of copper ion is 7.5-100mM, and the concentration of another metal ion is 0.1-10mM;
(3) in above-mentioned solution system, add reducing agent reduction, wherein reducing agent adds with the form of the aqueous solution, and the concentration of aqueous solution of reducing agent is 0.01-1M; Reducing agent consumption is 1-20 times of two kinds of metal component total mole numbers;
(4) reacted solution is carried out to centrifugation, the washing of solid nano material, obtain dendritic nano material.
4. preparation method according to claim 3, is characterized in that: surfactant used is nonionic surface active agent P123, F127, PVP, PVA, Triton X-100, Brij, Tergitol or Type15-s-7.
5. preparation method according to claim 3, is characterized in that: the mantoquita that described copper presoma is solubility, comprises one or two or more kinds in the complex of copper nitrate, copper chloride, copper sulphate, Schweinfurt green or copper.
6. preparation method according to claim 3, is characterized in that: another described metal precursor is the corresponding chloride of this metal, nitrate, sulfate or acetate.
7. preparation method according to claim 3, is characterized in that: reducing agent used is weak reductant, comprises ascorbic acid, formic acid, hydroxylamine hydrochloride, aldehyde compound or inferior sodium phosphate.
8. preparation method according to claim 3, is characterized in that: the dendritic nano material obtaining is distributed in water stand-by.
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