CN103143717A - Platinoid bimetallic nanometer material and preparation method and application thereof - Google Patents
Platinoid bimetallic nanometer material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a platinoid bimetallic nanometer material. The grain diameter of the material is 4-10 nanometers; the material has a multi-legged appearance; and the mole ratio of the platinoid is adjustable. The preparation method comprises the following steps of: filling soluble platinum precursor solution in 140-180 DEG C polyhydric alcohol thermal solution containing soluble copper precursor and little alkali liquor, and maintaining the temperature and stirring for 1-3 hours. The raw material of the preparation method is cheap and easy to obtain; the equipment technology is simple; and the yield is higher. The material has large potential application in the fields such as heterogeneous catalysis, electro-catalysis and photocatalysis, and particularly has excellent catalytic performance in the electro-catalysis.
Description
Technical field
The present invention relates to a kind of platinoid bimetal nano material and its preparation method and application.
Background technology
Platinum and bimetal nano catalyst thereof be due to its efficiently reduction and oxidation, and at heterogeneous catalysis, the application in photocatalysis and electro-catalysis field is very extensive.Except size, the pattern of platinum and double-metal nanocrystal thereof has also played crucial effect to the activity and selectivity of catalysis and electro-catalysis in reaction.The condition of modulation synthesizing single shape catalyst is as stabilizing agent, reducing agent and surfactant etc., most important for the pattern of regulation and control nano particle.Noble metal platinum is to provide the basic element of catalytic activity, and the practicality of platinum catalyst in the cost determination that reduces catalyst.The interpolation of copper not only can improve the activity and selectivity of catalyst, can also reduce production costs, so the controlledly synthesis of platinoid duplex metal nano granule and pattern thereof and application study is subject to domestic and international researcher's extensive concern.
Utilize the week reduction of polyalcohol to synthesize having difform Pt nanocrystal is a kind of important and classical method.The method is modal is with PVP as stabilizing agent, be dissolved in together with precursor in the alcoholic solution such as ethylene glycol, solvent is as the reaction of reducing agent.On the one hand PVP is as stabilizing agent, can prevent from that platinum particles from reuniting to grow up, on the other hand, by the protection of some crystal face being controlled the shape of nano particle.This method often is aided with metal or nonmetallic ion is accurately controlled nanocrystalline shape, as Fe
3+(referring to Han S B, Song Y J, Lee J M, et al.Electrochem.Commun., 2008,10:1044), Ag
+(referring to Song H, Kim F, Yang P D, et al.J.Phys.Chem.B, 2005,109:88) etc.Utilize these metals on some crystal face Characteristic Adsorption or reach with the redox reaction of platinum the purpose of controlling the crystal face speed of growth.The metals such as the Fe that is reduced, Ag can be removed by methods such as centrifugal, red fuming nitric acid (RFNA) etchings, can not introduce the interference of these metals.Difform Pt nanocrystal also can be achieved by changing reaction condition control reaction power mathematic(al) parameter.When rate of reduction was relatively very fast, nucleus was easy to form thermodynamically stable truncated octahedra shape; And rate of reduction is when slower, and the effect of stabilizing agent is more obvious.Herricks etc. find to add the NaNO of different amounts
3Can regulate the shape of the standby Pt nanocrystal of polyalcohol legal system, NaNO
3Can be reduced to nitrite and form stable complex compound with Pt (II) and Pt (IV), thereby reduce the rate of reduction of platinum, make the different crystal orientations growth rate of Pt nanocrystal change, the difform Pt nanocrystal of final generation is (referring to T.Herricks, J.Chen and Y.Xia, Nano Lett., 2004,4,2367).
Realize that with this classical way the pattern regulation and control of bimetallic platinoid rarely have report, and less than the synthetic of the platinoid bimetal nano particles of the polypody pattern of 10nm and use so far still without reporting.
Summary of the invention
The object of the present invention is to provide a kind of bimetal nano material and preparation and application;
For achieving the above object, the invention provides a kind of polypody shape platinoid bimetal nano material, this polypody shape (polypody shape: describe it as polypod or multipod in document) structure size 4-10nm, component ratio is controlled, and in the platinoid bimetallic, the platinoid molar ratio is 5: 1-1: 5.
Another purpose of the present invention is to provide a kind of method for preparing polypody shape platinoid bimetal nanostructure, and the method raw material is cheap and easy to get, and environmental friendliness is easy and simple to handle.
The preparation method of a kind of polypody shape platinoid bimetal nanostructure provided by the invention, its concrete steps are:
1) get polyhydric alcohol solutions, add PVP (polyvinylpyrrolidone) and a small amount of alkali lye (be less than 0.5ml, or do not add) of 1-10 times of platinum mole, add the soluble copper precursor, be heated to 140 ℃-180 ℃ under air or argon gas atmosphere;
2) the solubility platinum precursor aqueous solution is injected in the polyalcohol hot solution, kept this temperature stirring reaction 1-3 hour; Wherein the platinoid molar ratio is 1/10-10/1;
3) reaction was cooled to room temperature after 1-3 hour in hot solution, with acetone, nano particle was settled, and nano particle water and ethanol are washed PVP off.
Described polyalcohol is a kind of in ethylene glycol, 1,2-PD, 1,5-PD, diethylene glycol, triethylene glycol, tetraethylene glycol; Described PVP is that molecular weight is a kind of in 28k and 55k; Described alkali lye is to have a kind of in certain density NaOH, TMAH and the tetraethyl ammonium hydroxide aqueous solution;
Described solubility platinum precursor is a kind of in chloroplatinic acid and potassium chloroplatinate;
Described soluble copper precursor is a kind of in copper chloride and copper nitrate.
In described reaction system, the concentration of chloroplatinic acid root is 1-20mM.
Described nano material can be used as the electrocatalytic reaction that catalyst is used for fuel cell, has good electro catalytic activity.
Electrochemical test method to nano material provided by the invention is as follows:
The preparation of working electrode: take the rotating circular disk glass-carbon electrode as working electrode, the described nano material of claim 1 or 2 is dispersed in ethanolic solution, pipettes and spread upon in right amount on the glass disk electrode, coat again the Nafion ethanolic solution after ethanol evaporation.
Electro-chemical test: potentiodynamic method is adopted in the electrocatalysis characteristic test of platinoid bimetal nano material.Experimental system is three-electrode system, and the rotating circular disk that scribbles catalyst is working electrode, and platinum electrode is to electrode, Hg/Hg
2SO
4Be reference electrode.Electrolyte is HClO
4Solution.The electrokinetic potential sweep speed is 20 or 50mVs
-1Logical oxygen before test until in electrolyte oxygen reach capacity (25 ℃), continue logical appropriate oxygen and keep dissolved oxygen concentration, the rotating disk electrode (r.d.e) rotating speed is 500-2500r/min.
Description of drawings
Fig. 1 is transmission electron microscope (TEM) and the XRD of the embodiment of the present invention 1, the EDX result;
Fig. 2 is the transmission electron microscope photo of the embodiment of the present invention 2;
Fig. 3 is the transmission electron microscope photo of the embodiment of the present invention 3.
The specific embodiment
Embodiment 1:
Take 110mg PVP and join in the 25ml there-necked flask, add inwards 0.8ml125mMCuCl
2(AR) ethylene glycol solution, then add 8.55mL ethylene glycol, open simultaneously and stir, make its abundant mixed dissolution; Slowly being warming up to 160 ℃ in air atmosphere, keeping this temperature after 30 minutes, is the H of 77.3mM with concentration
2PtCl
6The solution of solution 0.65mL is injected into the CuCl that contains of 160 ℃
2The ethylene glycol hot solution in, stirring reaction 1 hour; Reacted solution is transferred in centrifuge tube, then add the long-pending acetone of triploid, 10000rpm centrifugation 5min, namely obtain platinoid polypody shape nanostructured, as Fig. 1, this polypody shape structure size is even, calculates the synthesizing nano-particle particle size 4.3nm of institute according to the XRD result by the Scherrer formula.
The nano particle that water and ethanol is washed is done EDX and ICP test and is obtained this nano particle and only contain Pt and two kinds of elements of Cu, and the PtCu ratio is 5/1.
Embodiment 2:
Take 110mg PVP and join in the 25ml there-necked flask, add inwards 0.8ml125mMCuCl
2(99.999%) ethylene glycol solution, then add 8.55mL ethylene glycol, open simultaneously and stir, make its abundant mixed dissolution; Slowly being warming up to 160 ℃ in air atmosphere, keeping this temperature after 30 minutes, is the H of 77.3mM with concentration
2PtCl
6The solution of solution 0.65mL is injected into the CuCl that contains of 160 ℃
2The ethylene glycol hot solution in, stirring reaction 1 hour; Reacted solution is transferred in centrifuge tube, then adds the long-pending acetone of triploid, 10000rpm centrifugation 5min namely obtains platinoid polypody shape nanostructured, and as Fig. 2, this polypody shape structure size is even.
The nano particle that water and ethanol is washed is done the ICP test, and to obtain this nano particle PtCu ratio be 3.7/1.
Embodiment 3:
Take 110mg PVP and join in the 25ml there-necked flask, add inwards 0.8ml125mMCuCl
2(99.999%) ethylene glycol solution, then add 8.55mL ethylene glycol, open simultaneously and stir, make its abundant mixed dissolution; Slowly being warming up to 160 ℃ in argon gas atmosphere, keeping this temperature after 30 minutes, is the H of 77.3mM with concentration
2PtCl
6The solution of solution 0.65mL is injected into the CuCl that contains of 160 ℃
2The ethylene glycol hot solution in, stirring reaction 1 hour; Reacted solution is transferred in centrifuge tube, then adds the long-pending acetone of triploid, 10000rpm centrifugation 5min namely obtains platinoid polypody shape nanostructured, and as Fig. 3, this polypody shape structure size is even.
The nano particle that water and ethanol is washed is done the ICP test, and to obtain this nano particle PtCu ratio be 2.5/1.
Embodiment 4:
Take 110mg PVP and join in the 25ml there-necked flask, add inwards 1.6m1125mMCuCl
2(AR) ethylene glycol solution, then add 7.75mL ethylene glycol, open simultaneously and stir, make its abundant mixed dissolution; Slowly being warming up to 160 ℃ under air atmosphere, keeping this temperature after 30 minutes, is the H of 77.3mM with concentration
2PtCl
6The solution of solution 0.65mL is injected into the CuCl that contains of 160 ℃
2The ethylene glycol hot solution in, stirring reaction 1 hour; Reacted solution is transferred in centrifuge tube, then adds the long-pending acetone of triploid, 10000rpm centrifugation 5min namely obtains platinoid polypody shape nanostructured, and by the Electronic Speculum picture as can be known, this polypody shape structure is obvious, and size evenly.
Embodiment 5:
Take 110mg PVP and join in the 25ml there-necked flask, add inwards 2.4ml125mMCuCl
2(99.999%) ethylene glycol solution, then add 6.95mL ethylene glycol, open simultaneously and stir, make its abundant mixed dissolution; Slowly being warming up to 160 ℃ under air atmosphere, keeping this temperature after 30 minutes, is the H of 77.3mM with concentration
2PtCl
6The solution of solution 0.65mL is injected into the CuCl that contains of 160 ℃
2The ethylene glycol hot solution in, stirring reaction 1 hour; Reacted solution is transferred in centrifuge tube, then adds the long-pending acetone of triploid, 10000rpm centrifugation 5min namely obtains platinoid polypody shape nanostructured, and by the Electronic Speculum picture as can be known, this polypody shape structure is obvious, and size evenly.
Embodiment 6:
Take 110mg PVP and join in the 25ml there-necked flask, add inwards 1.6ml125mMCuCl
2(99.999%) ethylene glycol solution, then add 7.75mL ethylene glycol, open simultaneously and stir, make its abundant mixed dissolution; Slowly being warming up to 180 ℃ under argon gas atmosphere, keeping this temperature after 30 minutes, is the H of 77.3mM with concentration
2PtCl
6The solution of solution 0.65mL is injected into the CuCl that contains of 180 ℃
2The ethylene glycol hot solution in, stirring reaction 1 hour; Reacted solution is transferred in centrifuge tube, then adds the long-pending acetone of triploid, 10000rpm centrifugation 5min namely obtains platinoid polypody shape nanostructured, and by the Electronic Speculum picture as can be known, platinoid bimetallic still major part is the polypody pattern, and size evenly.
Embodiment 7:
Take 110mg PVP and join in the 25ml there-necked flask, add inwards 1.6ml125mMCuCl
2(99.999%) ethylene glycol solution, then add 2.75mL ethylene glycol, open simultaneously and stir, make its abundant mixed dissolution; Slowly being warming up to 160 ℃ under argon gas atmosphere, keeping this temperature after 30 minutes, is the H of 77.3mM with concentration
2PtCl
6The solution of solution 0.65mL is injected into the CuCl that contains of 160 ℃
2The ethylene glycol hot solution in, stirring reaction 1 hour; Reacted solution is transferred in centrifuge tube, then adds the long-pending acetone of triploid, 10000rpm centrifugation 5min namely obtains platinoid polypody shape nanostructured, and by the Electronic Speculum picture as can be known, this polypody shape structure is obvious, and size evenly.
Embodiment 8:
Take 110mg PVP and join in the 25ml there-necked flask, add inwards 2.4ml125mMCuCl
2Ethylene glycol solution, then add 1.95mL ethylene glycol, open simultaneously and stir, make its abundant mixed dissolution; Slowly being warming up to 180 ℃ under argon gas atmosphere, keeping this temperature after 30 minutes, is the HPtCl of 77.3mM with concentration
6The solution of solution 0.65mL is injected into the CuCl that contains of 180 ℃
2The ethylene glycol hot solution in, stirring reaction 1 hour; Reacted solution is transferred in centrifuge tube, then adds the long-pending acetone of triploid, 10000rpm centrifugation 5min namely obtains platinoid polypody shape nanostructured, and by the Electronic Speculum picture as can be known, synthetic platinoid is more obvious polypody shape pattern, and size evenly.
Application examples:
The preparation of working electrode: take the rotating circular disk glass-carbon electrode as working electrode, the nano material that embodiment 1 is prepared is dispersed in quantitatively to 0.15 of ICP μ g μ L in ethanolic solution
-1, pipette 65.3 μ L and spread upon on the glass disk electrode, coat again 20 μ L mass fraction 0.025%Nafion ethanolic solutions after ethanol evaporation; The load capacity of platinum is 50 μ gcm
-2
Electro-chemical test: potentiodynamic method is adopted in the electrocatalysis characteristic test of platinoid bimetal nano material.Experimental system is three-electrode system, and the rotating circular disk that scribbles catalyst is working electrode, and platinum electrode is to electrode, Hg/Hg
2SO
4Be reference electrode.Electrolyte is 0.5molL
-1HClO
4Solution.The electrokinetic potential sweep speed is 20mVs
-1Logical oxygen before test until in electrolyte oxygen reach capacity (25 ℃), continue logical appropriate oxygen and keep dissolved oxygen concentration.
The electrochemical gaging instrument is chi 760 type potentiometers, and the rotating disk electrode (r.d.e) rotating speed is 1600r/min.
The electro-catalysis mass activity that is calculated the material of the prepared platinoid polypody shape structure of embodiment 1 by hydrogen reduction curve combined with electrochemical active area is: 15.4mAmg
Pt -1Business platinum black mass activity is 2.48mAmg under the same conditions
Pt -1With respect to platinum black, the prepared platinoid bimetal nano material of embodiment 1 is no matter mass activity or the intrinsic activity all is improved largely shows that it has good electro catalytic activity.
Claims (7)
1. platinoid bimetal nano material, it is characterized in that: particle diameter is 4-10nm, has polypody shape pattern.
2. nanostructured as claimed in claim 1, it is characterized in that: in the platinoid bimetallic, the platinoid molar ratio is 5: 1-1: 5.
3. the preparation method of the described nanostructured of claim 1, its preparation process is as follows:
1) get polyhydric alcohol solutions, add PVP (polyvinylpyrrolidone) and a small amount of alkali lye (be less than 0.5ml, or do not add) of 1-10 times of platinum mole, add the soluble copper precursor, be heated to 140 ℃-180 ℃ under air or argon gas atmosphere;
2) the solubility platinum precursor aqueous solution is injected in the polyalcohol hot solution, kept this temperature stirring reaction 1-3 hour; Wherein the platinoid molar ratio is 1/10-10/1;
3) reaction was cooled to room temperature after 1-3 hour in hot solution, with acetone, nano particle was settled, and nano particle water and ethanol are washed PVP off.
4. preparation method according to claim 3 is characterized in that:
Described polyalcohol is a kind of in ethylene glycol, 1,2-PD, 1,5-PD, diethylene glycol, triethylene glycol, tetraethylene glycol; Described PVP is that molecular weight is a kind of in 28k and 55k; Described alkali lye is to have a kind of in certain density NaOH, TMAH and the tetraethyl ammonium hydroxide aqueous solution;
Described solubility platinum precursor is a kind of in chloroplatinic acid and potassium chloroplatinate;
Described soluble copper precursor is a kind of in copper chloride and copper nitrate.
5. preparation method according to claim 3 is characterized in that:
In described reaction system, the concentration of chloroplatinic acid root is 1-20mM.
6. the application of claim 1 or 2 a described nanostructured is characterized in that:
The act as a fuel anode catalysis material of battery of described platinoid bimetal nano material.
7. the application of claim 1 or 2 a described nanostructured is characterized in that:
The preparation of working electrode: take the rotating circular disk glass-carbon electrode as working electrode, the described nano material of claim 1 or 2 is dispersed in ethanolic solution, pipettes and spread upon in right amount on the glass disk electrode, coat again the Nafion ethanolic solution after ethanol evaporation.
Electro-chemical test: potentiodynamic method is adopted in the electrocatalysis characteristic test of platinoid bimetal nano material.Experimental system is three-electrode system, and the rotating circular disk that scribbles catalyst is working electrode, and platinum electrode is to electrode, Hg/Hg
2SO
4Be reference electrode.Electrolyte is HClO
4Solution.The electrokinetic potential sweep speed is 20 or 50mVs
-1Logical oxygen before test until in electrolyte oxygen reach capacity (25 ℃), continue logical appropriate oxygen and keep dissolved oxygen concentration, the rotating disk electrode (r.d.e) rotating speed is 500-2500r/min.
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| CN104001521A (en) * | 2014-05-04 | 2014-08-27 | 昆明理工大学 | Carbon-supported PtCu alloy catalyst with controllable atomic concentration gradient and preparation method thereof |
| CN104759633A (en) * | 2015-03-03 | 2015-07-08 | 国家纳米科学中心 | Mimic enzyme, preparation method, application method and application of mimic enzyme |
| CN105363478A (en) * | 2015-10-10 | 2016-03-02 | 南京工程学院 | One-step solvothermal preparation method and application of M-doped Sex-Ru/C |
| CN105457654A (en) * | 2015-12-14 | 2016-04-06 | 厦门宇净环保科技有限公司 | Catalyst for removing formaldehyde through catalytic oxidation at indoor temperature and preparation method thereof |
| CN105478794A (en) * | 2015-12-11 | 2016-04-13 | 中国科学院深圳先进技术研究院 | Platinum-copper alloy nano particle and preparation method thereof |
| CN106732613A (en) * | 2017-01-11 | 2017-05-31 | 中国石油大学(华东) | A kind of preparation method of novel nano carbon material and its electro-catalysis hydrogen manufacturing application |
| CN107498066A (en) * | 2017-09-07 | 2017-12-22 | 浙江工业大学 | A kind of preparation method and applications of platinoid nano-material |
| CN108161025A (en) * | 2018-02-07 | 2018-06-15 | 中南民族大学 | A kind of eight foot-shape Pt-Cu alloy nano-materials and its synthetic method and application |
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| CN104001521A (en) * | 2014-05-04 | 2014-08-27 | 昆明理工大学 | Carbon-supported PtCu alloy catalyst with controllable atomic concentration gradient and preparation method thereof |
| CN104759633A (en) * | 2015-03-03 | 2015-07-08 | 国家纳米科学中心 | Mimic enzyme, preparation method, application method and application of mimic enzyme |
| CN105363478A (en) * | 2015-10-10 | 2016-03-02 | 南京工程学院 | One-step solvothermal preparation method and application of M-doped Sex-Ru/C |
| CN105478794A (en) * | 2015-12-11 | 2016-04-13 | 中国科学院深圳先进技术研究院 | Platinum-copper alloy nano particle and preparation method thereof |
| CN105457654A (en) * | 2015-12-14 | 2016-04-06 | 厦门宇净环保科技有限公司 | Catalyst for removing formaldehyde through catalytic oxidation at indoor temperature and preparation method thereof |
| CN105457654B (en) * | 2015-12-14 | 2018-06-19 | 厦门宇净环保科技有限公司 | Catalyst of room temperature catalytic oxidation removing formaldehyde and preparation method thereof |
| CN106732613A (en) * | 2017-01-11 | 2017-05-31 | 中国石油大学(华东) | A kind of preparation method of novel nano carbon material and its electro-catalysis hydrogen manufacturing application |
| CN107498066A (en) * | 2017-09-07 | 2017-12-22 | 浙江工业大学 | A kind of preparation method and applications of platinoid nano-material |
| CN108161025A (en) * | 2018-02-07 | 2018-06-15 | 中南民族大学 | A kind of eight foot-shape Pt-Cu alloy nano-materials and its synthetic method and application |
| CN109108303A (en) * | 2018-04-19 | 2019-01-01 | 哈尔滨理工大学 | A kind of preparation method of polymolecularity Pt-Cu alloy nanoparticle |
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Application publication date: 20130612 |