CN103352254B - The octahedra Mock gold of the preparation method that a kind of octahedra Mock gold is nanocrystalline and preparation thereof is nanocrystalline - Google Patents
The octahedra Mock gold of the preparation method that a kind of octahedra Mock gold is nanocrystalline and preparation thereof is nanocrystalline Download PDFInfo
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- CN103352254B CN103352254B CN201310282593.0A CN201310282593A CN103352254B CN 103352254 B CN103352254 B CN 103352254B CN 201310282593 A CN201310282593 A CN 201310282593A CN 103352254 B CN103352254 B CN 103352254B
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Abstract
The invention discloses the preparation method that a kind of octahedra Mock gold is nanocrystalline, adopt N, dinethylformamide (DMF) system and suitable dispersion agent, but do not quote other organic modifiers, also reductive agent is not introduced, only utilize the reductibility of DMF itself, hydro-thermal reaction 3 ~ 11h under 160 ~ 220 ° of C.Preparation method of the present invention is simple, and repeatability is high, and cost is low; The invention also discloses the octahedra Mock gold that described method prepares nanocrystalline, size be comparatively large, good dispersity and be easy to preserve, final product is scattered in alcohol and preserves.
Description
Technical field
The invention belongs to field of nanometer material technology, particularly relate to a kind of octahedra Mock gold nanocrystalline and preparation method thereof.
Background technology
In recent years, platinum group is nanocrystalline causes the great interest of people, the catalysis of their uniquenesses, electricity, sensing capabilities, and it is found application in many-side.But high price, limited store content limit again it and widely use.Address this problem at present, one of more successful way uses another kind of metal and platinum compound.The nanostructure of this compound, can reduce the usage quantity of platinum on the one hand, can bring more dominance energy in addition compared to pure platinum.
DMF (DMF) is well known with its excellent properties, comprising: range of reaction temperature is wide, excellent chemistry and thermostability, and polarity, dissolving power is better.These performances make it be applied in many-side: prepare colloid, organic chemical reactions etc.In the reaction, DMF not only plays the effect of solvent, more can play reductive action.Research finds under optimum conditions, and DMF will as reductive agent.
Nanocrystalline performance depends on many factors: composition, size, shape, structure, regulates these parameters, can design the nanocrystalline application in different field.People, by co-reducing process, thermolysis organometallic sources, electrochemical process, template, prepare the Pt-M(M=Fe of multiple high catalytic activity, Co, Ni, Cu, Mn, Ru, Au, Pd) nanocrystalline.As document HongzhouYang, JunZhang, KaiSun, ShouzhongZou, JiyeFang, J.Angew.Chem., 49 (2010), 6848-6851, the Pt prepared
3co alloy nanometer crystals has higher speed of reaction to oxygen reduction reaction.As YouXu, ShuangxiaHou, YangLiu, YueZhang, HuanWangandBinZhang, Chem.Commun., 48(2012), 2665-2667, the Pt prepared
3ni is nanocrystalline shows significantly improving direct methanol oxidation electro catalytic activity.But these methods need the complicated and reaction process of multistep and experiment condition strict, some reactions are difficult to accomplish scale production.
Summary of the invention
For the deficiencies in the prior art, the invention provides the preparation method that a kind of octahedra Mock gold is nanocrystalline, can obtain that size is relatively large, good dispersity octahedron nanocrystalline, and preparation method is simple, and repeatability is high, and cost is low.
The preparation method that octahedra Mock gold is nanocrystalline, comprises following steps:
(1) dispersion agent is dissolved in DMF, ultrasonic disperse 2 ~ 3min;
(2) the DMF solution in copper source and the DMF solution in platinum source are joined respectively in the solution that step (1) obtains;
(3) mixing solutions that step (2) obtains is joined in reactor, carry out hydro-thermal reaction;
(4) product step (3) obtained, through centrifugation, obtains described octahedra Mock gold nanocrystalline;
Described dispersion agent is polyvinylpyrrolidone, polyvinyl alcohol or polyoxyethylene glycol.
In 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 step (1) is polyvinylpyrrolidone, polyvinyl alcohol or polyoxyethylene glycol; Wherein polyvinylpyrrolidone has stronger coordination for transition-metal ions such as Au, Ag, Pt, show the stability of polyvinylpyrrolidone to metal, therefore, further preferred molecular weight is the polyvinylpyrrolidone (PVP) of 30000 ~ 55000, is more conducive to obtaining mono-dispersed nano brilliant.
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 one of this programme large feature is, except use dispersion agent, no longer add other promoting agents, as preferably, the copper source in step (2) is cupric chloride, cupric nitrate or copper sulfate; Platinum source is Platinic chloride, potassium platinichloride or sodium platinichloride.Research shows that halide-ions has a significant impact for the pattern of noble metal nanocrystalline, the present invention for obtaining octahedral pattern, the more preferably copper source of villaumite and platinum source.
Found by comparative study: the concentration in copper source and platinum source has a significant impact nanocrystalline pattern, when concentration is higher, the nanocrystalline output obtained is higher, but octahedra nanocrystalline size reduces, when concentration increases further, what obtain under similarity condition is nanocrystalline except size reduces, and particle agglomeration phenomenon is tending towards obvious.Therefore, for obtaining single dispersing, even, suitable nanocrystalline of size, as preferably, the N in copper source in step (2), in dinethylformamide solution, the concentration in copper source is 0.03 ~ 0.06mol/L, and in the DMF solution in platinum source, the concentration in platinum source is 0.019 ~ 0.058mol/L.
Because dispersion agent Main Function is in the present invention that to obtain dispersiveness nanocrystalline preferably, therefore the volume of consumption and the Tong Yuan of dispersion agent, platinum source and solvent for use is relevant.As preferably, the N in copper source, the N in dinethylformamide solution and platinum source, 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 building-up process that the octahedra Mock gold of the present invention is nanocrystalline, temperature is for the size important of particle, and particle size nanocrystalline is when the temperature is low less.As preferably, the hydrothermal reaction condition in step (3) is: 160 ~ 220 ° of C react 3 ~ 11h.
Present invention also offers the octahedra Mock gold that above-mentioned either method prepares 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, simple to operate, cost is lower, repeatability is high;
(2) the octahedra alloy nanometer crystals pattern, the dimensional homogeneity that obtain of the present invention is better;
(3) the present invention is easy to preparation and preserves, and final product is scattered in alcohol to be preserved.
Accompanying drawing explanation
Fig. 1 is the nanocrystalline transmission electron microscope photo of octahedra Mock gold that embodiment 1 obtains;
Fig. 2 is the octahedra Mock gold nanocrystalline transmission energy spectrogram that embodiment 1 obtains.
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) Platinic chloride (H is equipped with
2ptCl
6) and cupric chloride (CuCl
2) DMF solution, concentration is respectively 0.038mol/L and 0.05mol/L;
(2) by 0.18mol/L molecular weight be 30000 polyvinylpyrrolidone (PVP) join in 20mLDMF solvent, ultrasonic 2 ~ 3min dissolves;
(3) Platinic chloride prepared and Cupric Chloride Solution are added in (2) mixing solutions, the wherein volume ratio of copper source solution and platinum source solution: 6:1, the volume ratio of mixing solutions and the middle DMF solution of step (2) is 1:20, and ultrasonic 1 ~ 2min mixes;
(4) joined by the mixing solutions that (3) obtain in the water heating kettle of volume 40mL, 200 ° of C react 11h;
(5) the centrifugal 10min of rotating speed that the product (4) obtained turns through 12000-13000, abandoning supernatant, removes unnecessary PVP;
(6) the precipitation ultrasonic disperse (5) obtained is in ethanol, and normal temperature is preserved.
Fig. 1 and Fig. 2 is the nanocrystalline transmission electron microscope photo of the octahedra Mock gold that synthesized by the present embodiment and transmission energy spectrogram respectively.As seen from Figure 1, the octahedron that the present embodiment is comparatively homogeneous sized by obtaining is nanocrystalline.In Fig. 2, a ~ d part is the transmission energy spectrogram of 98000 multiplying powers; E ~ h is the transmission energy spectrogram of 260000 multiplying powers, and what be shown as copper and platinum from the transmission power spectrum of Fig. 2 can spectrogram be overlapping respectively the nanocrystalline power spectrum of octahedra Mock gold, thus demonstrates its alloying constituent.
Embodiment 2:
(1) Platinic chloride (H is equipped with
2ptCl
6) and cupric chloride (CuCl
2) DMF solution, concentration is respectively 0.045mol/L and 0.03mol/L;
(2) by 0.18mol/l molecular weight be 55000 polyoxyethylene glycol (PEG-2000) join in 20mLDMF solvent, ultrasonic 2 ~ 3min dissolves;
(3) potassium platinate prepared and Cupric Chloride Solution are added in (2) mixing solutions, the wherein volume ratio of copper source solution and platinum source solution: 4:1, the volume ratio of mixing solutions and the middle DMF solution of step (2) is 1:20, and ultrasonic 1 ~ 2min mixes;
(4) joined by the mixing solutions that (3) obtain in the water heating kettle of volume 40mL, 190 ° of C react 11h;
(5) the centrifugal 10min of rotating speed that the product (4) obtained turns through 12000-13000, abandoning supernatant, removes unnecessary PVP;
(6) the precipitation ultrasonic disperse (5) obtained is in ethanol, and normal temperature is preserved.The result obtained is similar to Example 1.
Embodiment 3:
(1) potassium platinichloride (K is equipped with
2ptCl
6) and cupric chloride (CuCl
2) DMF solution, concentration is respectively 0.05mol/L and 0.05mol/L;
(2) by 0.18mol/l molecular weight be 2000 polyoxyethylene glycol join in 20mlDMF solvent, ultrasonic 2 ~ 3min dissolves;
(3) potassium platinichloride prepared and Cupric Chloride Solution are added in (2) mixing solutions, the wherein volume ratio of copper source solution and platinum source solution: 3:1, in mixing solutions and step 2, the volume ratio of DMF solution is 1:25, and ultrasonic 1 ~ 2min mixes;
(4) joined by the mixing solutions that (3) obtain in the water heating kettle of volume 40mL, 180 ° of C react 11h;
(5) the centrifugal 10min of rotating speed that the product (4) obtained turns through 12000-13000, abandoning supernatant, removes unnecessary PEG;
(6) the precipitation ultrasonic disperse (5) obtained is in ethanol, and normal temperature is preserved.The result obtained is similar to Example 1.
Embodiment 4:
(1) potassium platinichloride (K is equipped with
2ptCl
6) and copper sulfate (CuSO
4) DMF solution, concentration is respectively 0.019mol/L and 0.03mol/L;
(2) join in 20mLDMF solvent by 0.18mol/l polyvinyl alcohol (PVA1795 type), ultrasonic 2 ~ 3min dissolves;
(3) potassium platinichloride prepared and copper-bath are added in (2) mixing solutions, the wherein volume ratio of copper source solution and platinum source solution: 12:1, in mixing solutions and step 2, the volume ratio of DMF solution is 1:20, and ultrasonic 1 ~ 2min mixes;
(4) joined by the mixing solutions that (3) obtain in the water heating kettle of volume 40mL, 220 ° of C react 11h;
(5) the centrifugal 10min of rotating speed that the product (4) obtained turns through 12000-13000, abandoning supernatant, removes unnecessary PVA;
(6) the precipitation ultrasonic disperse (5) obtained is in ethanol, and normal temperature is preserved.The result obtained is similar to Example 1.
Embodiment 5:
(1) sodium platinichloride (Na is equipped with
2ptCl
6) and cupric nitrate (Cu(NO
3)
2) DMF solution, concentration is respectively 0.038mol/L and 0.05mol/L;
(2) by 400mg molecular weight be 30000 PVP join in 20mLDMF solvent, ultrasonic 2 ~ 3min dissolves;
(3) sodium platinichloride prepared and copper nitrate solution are added in (2) mixing solutions, the wherein volume ratio of copper source solution and platinum source solution: 12:1, in mixing solutions and step 2, the volume ratio of DMF solution is 1:30, and ultrasonic 1 ~ 2min mixes;
(4) joined by the mixing solutions that (3) obtain in the water heating kettle of volume 40mL, 160 ° of C react 11h;
(5) the centrifugal 10min of rotating speed that the product (4) obtained turns through 12000-13000, abandoning supernatant, removes unnecessary PVP;
(6) the precipitation ultrasonic disperse (5) obtained is in ethanol, and normal temperature is preserved.The result obtained is similar to Example 1.
Embodiment 6:
(1) potassium platinichloride (K is equipped with
2ptCl
6) and copper sulfate (CuSO
4) DMF solution, concentration is respectively 0.05mol/L and 0.05mol/L;
(2) by 0.18mol/l molecular weight be 20000 polyoxyethylene glycol join in 20mlDMF solvent, ultrasonic 2 ~ 3min dissolves;
(3) potassium platinichloride prepared and copper-bath are added in (2) mixing solutions, the wherein volume ratio of copper source solution and platinum source solution: 3:1, in mixing solutions and step 2, the volume ratio of DMF solution is 1:20, and ultrasonic 1 ~ 2min mixes;
(4) joined by the mixing solutions that (3) obtain in the water heating kettle of volume 40mL, 180 ° of C react 11h;
(5) the centrifugal 10min of rotating speed that the product (4) obtained turns through 12000-13000, abandoning supernatant, removes unnecessary PEG-20000;
(6) the precipitation ultrasonic disperse (5) obtained is in ethanol, and normal temperature is preserved.
Embodiment 7:
(1) sodium platinichloride (Na is equipped with
2ptCl
6) and cupric nitrate (Cu(NO
3)
2) DMF solution, concentration is respectively 0.038mol/L and 0.05mol/L;
(2) by 400mg molecular weight be 30000 PVP join in 20mLDMF solvent, ultrasonic 2 ~ 3min dissolves;
(3) sodium platinichloride prepared and copper nitrate solution are added in (2) mixing solutions, the wherein volume ratio of copper source solution and platinum source solution: 6:1, in mixing solutions and step 2, the volume ratio of DMF solution is 1:25, and ultrasonic 1 ~ 2min mixes;
(4) joined by the mixing solutions that (3) obtain in the water heating kettle of volume 40mL, 160 ° of C react 11h;
(5) the centrifugal 10min of rotating speed that the product (4) obtained turns through 12000-13000, abandoning supernatant, removes unnecessary PVP;
(6) the precipitation ultrasonic disperse (5) obtained is in ethanol, and normal temperature is preserved.
Embodiment 8:
(1) Platinic chloride (H is equipped with
2ptCl
6) and cupric nitrate (Cu(NO
3)
2) DMF solution, concentration is respectively 0.038mol/L and 0.05mol/L;
(2) by 0.18mol/l molecular weight be 30000 polyvinylpyrrolidone (PVP) join in 20mLDMF solvent, ultrasonic 2 ~ 3min dissolves;
(3) Platinic chloride prepared and copper nitrate solution are added in (2) mixing solutions, the wherein volume ratio of copper source solution and platinum source solution: 4:1, in mixing solutions and step 2, the volume ratio of DMF solution is 1:20, and ultrasonic 1 ~ 2min mixes;
(4) joined by the mixing solutions that (3) obtain in the water heating kettle of volume 40mL, 220 ° of C react 11h;
(5) the centrifugal 10min of rotating speed that the product (4) obtained turns through 12000-13000, abandoning supernatant, removes unnecessary PVP;
(6) the precipitation ultrasonic disperse (5) obtained is in ethanol, and normal temperature is preserved.
Claims (3)
1. the preparation method that octahedra Mock gold is nanocrystalline, is characterized in that, comprises following steps:
(1) dispersion agent is dissolved in DMF, ultrasonic disperse 2 ~ 3min; The concentration of described dispersion agent is 0.14 ~ 0.28mol/L;
(2) the DMF solution in copper source and the DMF solution in platinum source are joined respectively in the solution that step (1) obtains; Described copper source is cupric chloride, cupric nitrate or copper sulfate; Platinum source is Platinic chloride, potassium platinichloride or sodium platinichloride;
(3) mixing solutions that step (2) obtains is joined in reactor, carry out hydro-thermal reaction; Hydrothermal reaction condition is: 160 ~ 220 DEG C of reaction 3 ~ 11h;
(4) product step (3) obtained, through centrifugation, obtains described octahedra Mock gold nanocrystalline;
Described dispersion agent is polyvinylpyrrolidone, polyvinyl alcohol or polyoxyethylene glycol.
2. the preparation method that octahedra Mock gold according to claim 1 is nanocrystalline, is characterized in that, in the DMF solution in the middle copper source of step (2), the concentration in copper source is 0.03 ~ 0.06mol/L; In the DMF solution in platinum source, the concentration in platinum source is 0.019 ~ 0.058mol/L.
3. the preparation method that octahedra Mock gold according to claim 2 is nanocrystalline, it is characterized in that, the N in copper source, the N in dinethylformamide solution and platinum source, 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.
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| CN104451782B (en) * | 2014-12-01 | 2017-08-25 | 上海师范大学 | A kind of octahedral structure nano platinum particle and its synthetic method and application |
| 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 |
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| 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 |
| CN106670503B (en) * | 2017-01-18 | 2018-05-25 | 北京化工大学 | A kind of preparation method of the platinoid nano particle of morphology controllable |
| CN106953103B (en) * | 2017-03-08 | 2019-04-09 | 济南大学 | A kind of monocrystalline gold@platinum nucleocapsid octahedron nanoparticle controllable method for preparing based on seed epitaxial growth |
| CN107755712B (en) * | 2017-10-26 | 2021-06-29 | 山东大学 | Method for preparing metal antimony powder |
| CN108161025B (en) * | 2018-02-07 | 2020-12-01 | 中南民族大学 | Octagon Pt-Cu alloy nano material and synthetic method and application thereof |
| 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 |
| CN110429287A (en) * | 2019-08-01 | 2019-11-08 | 贵州大学 | A kind of preparation and application of hollow PtCu octahedron alloy |
| CN113842910B (en) * | 2021-11-10 | 2022-08-30 | 江南大学 | Chiral Pt @ Au material and preparation method and application thereof |
| CN115446303B (en) * | 2022-09-16 | 2024-01-16 | 中国人民解放军国防科技大学 | Platinum quantum dot and simple preparation method and application thereof |
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