CN103352254A - Method for preparing octahedral platinoid alloy nanocrystals and octahedral platinoid alloy nanocrystal prepared through adopting same - Google Patents
Method for preparing octahedral platinoid alloy nanocrystals and octahedral platinoid alloy nanocrystal prepared through adopting same Download PDFInfo
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- CN103352254A CN103352254A CN2013102825930A CN201310282593A CN103352254A CN 103352254 A CN103352254 A CN 103352254A CN 2013102825930 A CN2013102825930 A CN 2013102825930A CN 201310282593 A CN201310282593 A CN 201310282593A CN 103352254 A CN103352254 A CN 103352254A
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Abstract
The invention discloses a method for preparing octahedral platinoid alloy nanocrystals. In the method, an N,N-dimethylformamide (DMF) system and appropriate dispersing agent are adopted, other organic modifier and reducing agent are not introduced, only the reducibility of the DMF is utilized, and the hydrothermal reaction for 3-11 h at the temperature of 160-220 DEG C is performed. The preparing method is simple, high in repeatability and low in cost. The invention further discloses an octahedral platinoid alloy nanocrystal obtained and prepared through the method, and the octahedral platinoid alloy nanocrystal is larger in size, excellent in dispersity and easy to store, and the end product can be dispersed in ethyl alcohol and stored.
Description
Technical field
The invention belongs to field of nanometer material technology, it is nanocrystalline and preparation method thereof to relate in particular to a kind of octahedra Mock gold.
Background technology
In recent years, the nanocrystalline great interest of people that caused of platinum group, the catalysis of their uniquenesses, electricity, sensing capabilities are so that it finds application in many-side.But high price, limited store content limit again it and are widely used.Address this problem at present, one of more successful way is that the another kind of metal of use and platinum are compound.This compound nanostructure, one side can reduce the usage quantity of platinum, can bring more dominance energy compared to pure platinum in addition.
DMF (DMF) is well known with its excellent properties, comprising: range of reaction temperature is wide, good chemistry and thermostability, and polarity, dissolving power is better.These performances so that its be applied in many-side: preparation colloid, organic chemical reactions etc.In reaction, DMF not only plays the effect of solvent, more can play reductive action.Research finds that under optimum conditions DMF will be as reductive agent.
Nanocrystalline performance depends on many factors: composition, size, shape, structure, regulate these parameters, and can design nanocrystalline application in different field.People prepare the Pt-M(M=Fe of multiple high catalytic activity, Co, Ni, Cu, Mn, Ru, Au, Pd by co-reducing process, thermolysis organometallic sources, electrochemical process, template) nanocrystalline.Such as document Hongzhou Yang, Jun Zhang, Kai Sun, Shouzhong Zou, Jiye Fang, J.Angew.Chem., 49 (2010), 6848-6851, the Pt for preparing
3The Co alloy nanometer crystals has higher speed of reaction to oxygen reduction reaction.Such as You Xu, Shuangxia Hou, Yang Liu, Yue Zhang, Huan Wang and Bin Zhang, Chem.Commun., 48(2012), 2665-2667, the Pt for preparing
3The nanocrystalline obvious raising that has shown direct Electrocatalytic Oxidation of Methanol activity of Ni.But these methods need the reaction process of complexity and multistep and experiment condition strict, and some reactions are difficult to accomplish scale production.
Summary of the invention
For the deficiencies in the prior art, the invention provides the nanocrystalline preparation method of a kind of octahedra Mock gold, can make that size is relatively large, good dispersity octahedra nanocrystalline, and the preparation method is simple, repeatability is high, cost is low.
The nanocrystalline preparation method of a kind of octahedra Mock gold comprises following steps:
(1) dispersion agent is dissolved in the DMF ultra-sonic dispersion 2～3min;
(2) the DMF solution in the DMF solution in copper source and platinum source is joined respectively in the solution that step (1) obtains;
(3) mixing solutions that step (2) is obtained joins in the reactor, carries out hydro-thermal reaction;
(4) product that step (3) is obtained is through centrifugation, and it is nanocrystalline to obtain described octahedra Mock gold;
Described dispersion agent is polyvinylpyrrolidone, polyvinyl alcohol or polyoxyethylene glycol.
Among the present invention, the Main Function of dispersion agent is that to obtain mono-dispersed nano brilliant, and as preferably, in the solution of step (1), the concentration of dispersion agent is 0.14～0.28mol/L.
Dispersion agent in the step (1) is polyvinylpyrrolidone, polyvinyl alcohol or polyoxyethylene glycol; Wherein polyvinylpyrrolidone has stronger coordination for transition-metal ions such as Au, Ag, Pt, shown the stability of polyvinylpyrrolidone to metal, therefore, further preferred molecular weight is 30000～55000 polyvinylpyrrolidone (PVP), more is conducive to obtain the mono-dispersed nano crystalline substance.
The present invention is that the octahedra Mock gold of middle preparation is nanocrystalline in DMF (DMF) system, and wherein DMF is solvent, is again reductive agent.Therefore, the selection of raw material must be to be dissolved in DMF solution, and large characteristics of this programme are, except using dispersion agent, no longer adds other promoting agents, and as preferably, the copper source in the step (2) is cupric chloride, cupric nitrate or copper sulfate; The platinum source is Platinic chloride, potassium platinichloride or sodium platinichloride.Studies show that halide-ions has a significant impact for the pattern of noble metal nanocrystalline, the present invention is for obtaining octahedral pattern, more preferably the copper source of villaumite and platinum source.
Find by comparative study: the concentration in copper source and platinum source has a significant impact nanocrystalline pattern, when concentration is higher, the nanocrystalline output that obtains is higher, but octahedra nanocrystalline size reduction, when concentration further increases, what obtain under similarity condition is nanocrystalline except size reduction, and it is obvious that the particle agglomeration phenomenon is tending towards.Therefore, for obtaining single dispersion, even, suitable nanocrystalline of size, as preferably, the N in copper source in the step (2), the concentration in copper source is 0.03～0.06mol/L in the dinethylformamide solution, and the concentration in platinum source is 0.019～0.058mol/L in the DMF solution in platinum source.
Because dispersion agent Main Function in the present invention is that the acquisition dispersiveness is nanocrystalline preferably, so the consumption of dispersion agent is relevant with the volume of Tong Yuan, platinum source and solvent for use.As preferably, the N in copper source, the N in dinethylformamide solution and platinum source, the dinethylformamide liquor capacity is than being 12:1～1:6, the N in copper source, the volume ratio of the solution that the cumulative volume of the DMF solution in dinethylformamide solution and platinum source and step (1) obtain is 0.5～1:20.
In the nanocrystalline building-up process of the octahedra Mock gold of the present invention, temperature is for the big or small important of particle, and particle size nanocrystalline when temperature is low is less.As preferably, the hydrothermal reaction condition in the step (3) is: 160～220 ° of C reaction 3～11h.
The octahedra Mock gold that the present invention also provides above-mentioned either method to prepare is nanocrystalline.
Compared with prior art, the present invention has following beneficial effect:
(1) the present invention does not introduce other organic modifiers except dispersion agent, does not introduce reductive agent yet, only utilizes the reductibility of DMF itself, and is simple to operate, cost is lower, repeatability is high;
(2) the octahedra alloy nanometer crystals pattern, the dimensional homogeneity that make of the present invention is better;
(3) the present invention is easy to preparation and preserves, and final product is scattered in to preserve in the alcohol and gets final product.
Description of drawings
Fig. 1 is the nanocrystalline transmission electron microscope photo of octahedra Mock gold that embodiment 1 obtains;
Fig. 2 is that the nanocrystalline transmission of octahedra Mock gold that embodiment 1 obtains can spectrogram.
Embodiment
Describe the present invention in detail below in conjunction with embodiment and accompanying drawing, but the present invention is not limited to this.
Embodiment 1:
(1) is equipped with Platinic chloride (H
2PtCl
6) and cupric chloride (CuCl
2) DMF solution, concentration is respectively 0.038mol/L and 0.05mol/L;
(2) be that 30000 polyvinylpyrrolidone (PVP) joins in the 20mL DMF solvent with the 0.18mol/L molecular weight, ultrasonic 2～3min dissolving;
(3) Platinic chloride for preparing and Cupric Chloride Solution are added in (2) mixing solutions, the volume ratio of copper source solution and platinum source solution: 6:1 wherein, the volume ratio of the middle DMF solution of mixing solutions and step (2) is 1:20, ultrasonic 1～2min mixes;
(4) mixing solutions that (3) is obtained joins in the water heating kettle of volume 40mL, 200 ° of C reaction 11h;
(5) the centrifugal 10min of rotating speed that the product that (4) is obtained turns through 12000-13000, abandoning supernatant is removed unnecessary PVP;
(6) the precipitation ultra-sonic dispersion that (5) is obtained is in ethanol, and normal temperature is preserved.
Fig. 1 and Fig. 2 are respectively can spectrogram by the synthetic octahedra Mock gold of present embodiment nanocrystalline transmission electron microscope photo and transmission.What as seen from Figure 1, present embodiment obtained is the octahedra nanocrystalline of big or small comparatively homogeneous.A～d partly is the transmission energy spectrogram of 98000 multiplying powers among Fig. 2; E～h is that the transmission of 260000 multiplying powers can spectrogram, and what be shown as copper and platinum from the transmission power spectrum of Fig. 2 can spectrogram be overlapping the nanocrystalline power spectrum of octahedra Mock gold respectively, thereby has proved its alloying constituent.
Embodiment 2:
(1) is equipped with Platinic chloride (H
2PtCl
6) and cupric chloride (CuCl
2) DMF solution, concentration is respectively 0.045mol/L and 0.03mol/L;
(2) be that 55000 polyoxyethylene glycol (PEG-2000) joins in the 20mL DMF solvent with the 0.18mol/l molecular weight, ultrasonic 2～3min dissolving;
(3) potassium platinate for preparing and Cupric Chloride Solution are added in (2) mixing solutions, the volume ratio of copper source solution and platinum source solution: 4:1 wherein, the volume ratio of the middle DMF solution of mixing solutions and step (2) is 1:20, ultrasonic 1～2min mixes;
(4) mixing solutions that (3) is obtained joins in the water heating kettle of volume 40mL, 190 ° of C reaction 11h;
(5) the centrifugal 10min of rotating speed that the product that (4) is obtained turns through 12000-13000, abandoning supernatant is removed unnecessary PVP;
(6) the precipitation ultra-sonic dispersion that (5) is obtained is in ethanol, and normal temperature is preserved.The result who obtains is similar to Example 1.
Embodiment 3:
(1) is equipped with potassium platinichloride (K
2PtCl
6) and cupric chloride (CuCl
2) DMF solution, concentration is respectively 0.05mol/L and 0.05mol/L;
(2) be that 2000 polyoxyethylene glycol joins in the 20ml DMF solvent with the 0.18mol/l molecular weight, ultrasonic 2～3min dissolving;
(3) potassium platinichloride for preparing and Cupric Chloride Solution are added in (2) mixing solutions, the volume ratio of copper source solution and platinum source solution: 3:1 wherein, the volume ratio of DMF solution is 1:25 in mixing solutions and the step 2, ultrasonic 1～2min mixes;
(4) mixing solutions that (3) is obtained joins in the water heating kettle of volume 40mL, 180 ° of C reaction 11h;
(5) the centrifugal 10min of rotating speed that the product that (4) is obtained turns through 12000-13000, abandoning supernatant is removed unnecessary PEG;
(6) the precipitation ultra-sonic dispersion that (5) is obtained is in ethanol, and normal temperature is preserved.The result who obtains is similar to Example 1.
Embodiment 4:
(1) is equipped with potassium platinichloride (K
2PtCl
6) and copper sulfate (CuSO
4) DMF solution, concentration is respectively 0.019mol/L and 0.03mol/L;
(2) 0.18mol/l polyvinyl alcohol (PVA1795 type) is joined in the 20mL DMF solvent ultrasonic 2～3min dissolving;
(3) potassium platinichloride for preparing and copper-bath are added in (2) mixing solutions, the volume ratio of copper source solution and platinum source solution: 12:1 wherein, the volume ratio of DMF solution is 1:20 in mixing solutions and the step 2, ultrasonic 1～2min mixes;
(4) mixing solutions that (3) is obtained joins in the water heating kettle of volume 40mL, 220 ° of C reaction 11h;
(5) the centrifugal 10min of rotating speed that the product that (4) is obtained turns through 12000-13000, abandoning supernatant is removed unnecessary PVA;
(6) the precipitation ultra-sonic dispersion that (5) is obtained is in ethanol, and normal temperature is preserved.The result who obtains is similar to Example 1.
Embodiment 5:
(1) is equipped with sodium platinichloride (Na
2PtCl
6) and cupric nitrate (Cu(NO
3)
2) DMF solution, concentration is respectively 0.038mol/L and 0.05mol/L;
(2) be that 30000 PVP joins in the 20mL DMF solvent with the 400mg molecular weight, ultrasonic 2～3min dissolving;
(3) sodium platinichloride for preparing and copper nitrate solution are added in (2) mixing solutions, the volume ratio of copper source solution and platinum source solution: 12:1 wherein, the volume ratio of DMF solution is 1:30 in mixing solutions and the step 2, ultrasonic 1～2min mixes;
(4) mixing solutions that (3) is obtained joins in the water heating kettle of volume 40mL, 160 ° of C reaction 11h;
(5) the centrifugal 10min of rotating speed that the product that (4) is obtained turns through 12000-13000, abandoning supernatant is removed unnecessary PVP;
(6) the precipitation ultra-sonic dispersion that (5) is obtained is in ethanol, and normal temperature is preserved.The result who obtains is similar to Example 1.
Embodiment 6:
(1) is equipped with potassium platinichloride (K
2PtCl
6) and copper sulfate (CuSO
4) DMF solution, concentration is respectively 0.05mol/L and 0.05mol/L;
(2) be that 20000 polyoxyethylene glycol joins in the 20ml DMF solvent with the 0.18mol/l molecular weight, ultrasonic 2～3min dissolving;
(3) potassium platinichloride for preparing and copper-bath are added in (2) mixing solutions, the volume ratio of copper source solution and platinum source solution: 3:1 wherein, the volume ratio of DMF solution is 1:20 in mixing solutions and the step 2, ultrasonic 1～2min mixes;
(4) mixing solutions that (3) is obtained joins in the water heating kettle of volume 40mL, 180 ° of C reaction 11h;
(5) the centrifugal 10min of rotating speed that the product that (4) is obtained turns through 12000-13000, abandoning supernatant is removed unnecessary PEG-20000;
(6) the precipitation ultra-sonic dispersion that (5) is obtained is in ethanol, and normal temperature is preserved.
Embodiment 7:
(1) is equipped with sodium platinichloride (Na
2PtCl
6) and cupric nitrate (Cu(NO
3)
2) DMF solution, concentration is respectively 0.038mol/L and 0.05mol/L;
(2) be that 30000 PVP joins in the 20mL DMF solvent with the 400mg molecular weight, ultrasonic 2～3min dissolving;
(3) sodium platinichloride for preparing and copper nitrate solution are added in (2) mixing solutions, the volume ratio of copper source solution and platinum source solution: 6:1 wherein, the volume ratio of DMF solution is 1:25 in mixing solutions and the step 2, ultrasonic 1～2min mixes;
(4) mixing solutions that (3) is obtained joins in the water heating kettle of volume 40mL, 160 ° of C reaction 11h;
(5) the centrifugal 10min of rotating speed that the product that (4) is obtained turns through 12000-13000, abandoning supernatant is removed unnecessary PVP;
(6) the precipitation ultra-sonic dispersion that (5) is obtained is in ethanol, and normal temperature is preserved.
Embodiment 8:
(1) is equipped with Platinic chloride (H
2PtCl
6) and cupric nitrate (Cu(NO
3)
2) DMF solution, concentration is respectively 0.038mol/L and 0.05mol/L;
(2) be that 30000 polyvinylpyrrolidone (PVP) joins in the 20mL DMF solvent with the 0.18mol/l molecular weight, ultrasonic 2～3min dissolving;
(3) Platinic chloride for preparing and copper nitrate solution are added in (2) mixing solutions, the volume ratio of copper source solution and platinum source solution: 4:1 wherein, the volume ratio of DMF solution is 1:20 in mixing solutions and the step 2, ultrasonic 1～2min mixes;
(4) mixing solutions that (3) is obtained joins in the water heating kettle of volume 40mL, 220 ° of C reaction 11h;
(5) the centrifugal 10min of rotating speed that the product that (4) is obtained turns through 12000-13000, abandoning supernatant is removed unnecessary PVP;
(6) the precipitation ultra-sonic dispersion that (5) is obtained is in ethanol, and normal temperature is preserved.
Claims (7)
1. the preparation method that octahedra Mock gold is nanocrystalline is characterized in that, comprises following steps:
(1) dispersion agent is dissolved in the DMF ultra-sonic dispersion 2～3min;
(2) the DMF solution in the DMF solution in copper source and platinum source is joined respectively in the solution that step (1) obtains;
(3) mixing solutions that step (2) is obtained joins in the reactor, carries out hydro-thermal reaction;
(4) product that step (3) is obtained is through centrifugation, and it is nanocrystalline to obtain described octahedra Mock gold;
Described dispersion agent is polyvinylpyrrolidone, polyvinyl alcohol or polyoxyethylene glycol.
2. the nanocrystalline preparation method of octahedra Mock gold according to claim 1 is characterized in that, in the solution of step (1), the concentration of dispersion agent is 0.14～0.28mol/L.
3. the nanocrystalline preparation method of octahedra Mock gold according to claim 1 is characterized in that, the copper source in the step (2) is cupric chloride, cupric nitrate or copper sulfate; The platinum source is Platinic chloride, potassium platinichloride or sodium platinichloride.
4. the nanocrystalline preparation method of octahedra Mock gold according to claim 1 is characterized in that, the concentration in copper source is 0.03～0.06mol/L in the DMF solution in the middle copper source of step (2); The concentration in platinum source is 0.019～0.058mol/L in the DMF solution in platinum source.
5. the nanocrystalline preparation method of octahedra Mock gold according to claim 4, it is characterized in that, the N in copper source, the N in dinethylformamide solution and platinum source, the dinethylformamide liquor capacity is than being 12:1～1:6, the volume ratio of the solution that the cumulative volume of the DMF solution in copper source and the DMF solution in platinum source and step (1) obtain is 0.5～1:20.
6. the nanocrystalline preparation method of octahedra Mock gold according to claim 1 is characterized in that, the hydrothermal reaction condition in the step (3) is: 160～220 ° of C reaction 3～11h.
7. the octahedra Mock gold for preparing of arbitrary claim is nanocrystalline according to claim 1～6.
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| CN103668462A (en) * | 2013-11-27 | 2014-03-26 | 浙江大学 | Preparation method of platinum-palladium alloy nanocrystalline |
| CN104451782A (en) * | 2014-12-01 | 2015-03-25 | 上海师范大学 | Octahedral platinum nanoparticles as well as synthesis method and application 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 |
| CN105887196A (en) * | 2016-04-15 | 2016-08-24 | 中国科学技术大学先进技术研究院 | Pt3Co nanocrystal, catalyst, preparation methods of Pt3Co nanocrystal and catalyst as well as application of catalyst |
| CN106493386A (en) * | 2016-11-03 | 2017-03-15 | 国家纳米科学中心 | The octahedral shape Nanoalloy of octahedra Nanoalloy and porous, Preparation Method And The Use |
| CN106505215A (en) * | 2017-01-09 | 2017-03-15 | 贵州大学 | A kind of synthetic method of the octahedral PtCu nanocrystals of sub- 5 nanometers of rescinded angles |
| CN106670503A (en) * | 2017-01-18 | 2017-05-17 | 北京化工大学 | Preparation method for platinum-copper nano-particles with controllable morphologies |
| CN106953103A (en) * | 2017-03-08 | 2017-07-14 | 济南大学 | A kind of octahedra nano-particle controllable method for preparing of the monocrystalline gold@platinum nucleocapsid based on seed epitaxial growth |
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| CN109261979A (en) * | 2018-11-19 | 2019-01-25 | 嘉兴学院 | A kind of preparation method of platinum-gold nanocages and its application in the catalyst |
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| CN103668462A (en) * | 2013-11-27 | 2014-03-26 | 浙江大学 | Preparation method of platinum-palladium alloy nanocrystalline |
| CN103668462B (en) * | 2013-11-27 | 2016-03-30 | 浙江大学 | A kind of preparation method of platinum-palladium alloy nanocrystalline |
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| CN106953103A (en) * | 2017-03-08 | 2017-07-14 | 济南大学 | A kind of octahedra nano-particle controllable method for preparing of the monocrystalline gold@platinum nucleocapsid based on seed epitaxial growth |
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| CN109261979A (en) * | 2018-11-19 | 2019-01-25 | 嘉兴学院 | A kind of preparation method of platinum-gold nanocages and its application in the catalyst |
| CN109261979B (en) * | 2018-11-19 | 2021-06-08 | 嘉兴学院 | Preparation method of platinum-gold nanocages and application of platinum-gold nanocages in catalyst |
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