CN104190921A - Nano particle of Au/Ni12P5 nuclear shell structure and preparation method thereof - Google Patents

Nano particle of Au/Ni12P5 nuclear shell structure and preparation method thereof Download PDF

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CN104190921A
CN104190921A CN201410443538.XA CN201410443538A CN104190921A CN 104190921 A CN104190921 A CN 104190921A CN 201410443538 A CN201410443538 A CN 201410443538A CN 104190921 A CN104190921 A CN 104190921A
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王荣明
段嗣斌
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University of Science and Technology Beijing USTB
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Abstract

The invention discloses a nano particle of an Au/Ni12P5 nuclear shell structure. The nano particle is composed of a face-centered cubic phase Au shell and a body-centered tetragonal phase Ni12P5 shell layer, and the Ni12P5 shell layer is of a single-crystal structure. A preparation method of the nano particle is a method of in-situ transformation combined with recrystallization and comprises the steps that an Au-Ni dumbbell structure which is synthetized in advance is used as a precursor body, triphenylphosphine is added, and the Au-Ni dumbbell structure is converted into an Au-Ni12P5 nuclear shell structure in an in-situ mode. The method provides a way capable of effectively preparing a novel metal-semiconductor nuclear shell structure nano material with a single crystal semiconductor shell layer, operation is easy, and product homogeneity is good. The obtained nano particle of the Au/Ni12P5 nuclear shell structure has very good stability and physical physicochemical property, the excellent capacitive performance can provide a good foundation in application of electrochemistry energy storage devices with high energy density and high charge and discharge stability, and the nano particle can be widely applied to the fields of supercapacitors, catalysts and the like.

Description

A kind of Au/Ni 12p 5nano particle of nucleocapsid structure and preparation method thereof
Technical field
The present invention relates to metal-semiconductor composite nano materials, be specifically related to a kind of Au/Ni with monocrystalline shell 12p 5nano particle of nucleocapsid structure and preparation method thereof.
Background technology
In recent years, nano materials research is the focus of scientific research always.Semiconductor nano material, compared to its block materials, due to small-size effect, skin effect etc., there are more horn of plenty and good physicochemical properties, in many research fields such as energy conversion, nanocomposite optical, heterogeneous catalysis, photoelectronics and medical diagnosis, have very important application prospect.But along with scientific and technical progress, the semiconductor nano material of one-component is also difficult to meet multifunction and intelligentized actual needs in performance.For this reason, on nanometer, atomic scale, to multiple semiconductor, be that the micro-structural of basic composite construction particle and component design and cut out be the important directions of current nano materials research.
Metal-semiconductor composite construction nano material is due to synergistic existence between metal-semiconductor, can realize the orientation optimizes to semi-conducting material particular characteristic, widen its application, at numerous areas such as electronics, catalysis, the energy, there is important application, attracted numerous scientists' research interest.Main and its interface of synergy between metal and semiconductor is closely related.Core-shell structured nanomaterials has controlled surface and interface, is considered to one of the most promising composite construction.The metal-semiconductor nucleocapsid structure especially with single crystal semiconductor shell has not only been widened the research category of Semiconductor Physics and nanometer technology, and due to the physical and chemical performance of its enhancing, for semiconductor nano material device provides the foundation.But because the interface energy between metal and semiconductor is larger, make semiconductor tend to spontaneous nucleation rather than be attached to nucleation on metal nanoparticle, cause semiconductor can not be wrapped in equably metal nanoparticle surface.The accurate controlledly synthesis of metal-semiconductor compound core-shell nano structure still faces very large challenge.
The method of the synthetic metal-semiconductor composite construction nano particle using is at present mainly " seed mediated growth method ".The method is in prior synthetic metal nano material surface second growing semiconductor nano material, thereby form metal-semiconductor composite construction, but the method forms nucleocapsid structure that nucleocapsid structure especially has monocrystalline shell, require to there is similar crystal structure (General Requirements lattice paprmeter difference <10%) between metal and semiconductor.
It is complicated that the preparation method of traditional metal-semiconductor core-shell structured nanomaterials exists preparation system, and the semiconductor shell of preparation exists the shortcomings such as crystal defect, monocrystalline be bad.
Summary of the invention
The object of the present invention is to provide a kind of semiconductor shell is monocrystalline, the having good uniformity of nano particle, excellent performance and have the metal-semiconductor composite nano materials of good stability; Be Au/Ni 12p 5core-shell nano.Another object of the present invention is to provide the Au/Ni with monocrystalline shell 12p 5the preparation method of core-shell nano, this preparation method has overcome the deficiencies such as the required technique of prior art and system are complicated, crystal structure requirement is harsh, shell monocrystalline is bad.
For achieving the above object, the present invention is by the following technical solutions:
A kind of Au/Ni 12p 5core-shell structure nanometer particle wherein, is face-centered cubic phase Au and body-centered tetragonal phase Ni 12p 5, golden nickle atom ratio is 8:92～15:85, Au/Ni 12p 5the diameter of core-shell nano structure is at 15nm～30nm, and Au nuclear diameter is 5nm～10nm; Semiconductor N i 12p 5shell is mono-crystalline structures.
A kind of synthetic Au/Ni 12p 5the method of the nano particle of nucleocapsid structure, is characterized in that, the method comprises:
(1), preparation Au nano particle: utilize the mixed solution of oleyl amine and nickel acetylacetonate as raw material, add chlorauric acid solution, obtain the oleyl amine solution containing the nickel acetylacetonate of Au nano particle after reaction;
(2), preparation Au-Ni dumbbell structure nano particle: the oleyl amine solution of the nickel acetylacetonate containing Au nano particle that described step (1) is obtained heats up, and obtains Au-Ni dumbbell structure nanoparticles solution after reaction;
(3), converted in-situ: obtain in described Au-Ni dumbbell structure nanoparticles solution and add triphenylphosphine in step (2), after continuing to heat up, reaction obtains Au/Ni 12p 5the solution of core-shell structure nanometer particle;
(4), separation cleaning: by described Au/Ni 12p 5the separated Au/Ni that obtains of solution of core-shell structure nanometer particle 12p 5core-shell structure nanometer particle.
Method as mentioned above; preferably, at the solvent of chlorauric acid solution described in step (1), be toluene, the reaction condition of described acquisition Au nano-particle solution is to be connected with under the condition of the protective gas such as nitrogen or argon gas; reaction temperature is 100 ℃, and the reaction time is 10min at least.
Method, preferably, obtains the reaction condition of Au-Ni dumbbell structure nanoparticles solution for being 230 ℃ in temperature in described step (2) as mentioned above, reacts at least 60min.
Method as mentioned above, preferably, the reaction condition of converted in-situ described in described step (3), for being 270 ℃～320 ℃ in temperature, reacts at least 60min.
Method as mentioned above, preferably, Au/Ni in described step (4) 12p 5the solution process centrifugation of core-shell structure nanometer particle, then pass through acetone ultrasonic cleaning, obtain the Au/Ni with monocrystalline shell 12p 5the nano particle of nucleocapsid structure.
Method as mentioned above, preferably, the centrifuge speed of described centrifugation is 10000rpm～15000rpm, centrifugation time is 10min.
Method as mentioned above, preferably, the ultrasonic wave of described ultrasonic cleaning is 50MHz～100MHz, wash number is at least 3 times.
Method as mentioned above, synthetic Au/Ni 12p 5the nano particle of nucleocapsid structure is face-centered cubic phase Au core and body-centered tetragonal phase Ni 12p 5shell forms, and wherein, golden nickle atom ratio is 8:92～15:85, described Au/Ni 12p 5the diameter of core-shell structure nanometer particle is at 15nm～30nm, and described Au nuclear diameter is 5nm～10nm; Described Ni 12p 5shell is mono-crystalline structures.
Au/Ni described above 12p 5the application of the nano particle of nucleocapsid structure in super capacitor material.
Au/Ni of the present invention 12p 5pattern, the dimensional homogeneity of core-shell structure nanometer particle are good, and semiconductor shell is monocrystalline, and excellent performance and have good stability is better than electric capacity.
Preparation Au/Ni provided by the invention 12p 5the controllable synthesis method of core-shell nano structure, is to adopt converted in-situ in conjunction with the method for recrystallization, and the synthetic in advance Au-Ni dumbbell structure of take is presoma, adds triphenylphosphine, by Au-Ni dumbbell structure converted in-situ, is Au/Ni 12p 5nucleocapsid structure, it has the semiconductor shell of monocrystalline.
The method batching cost used is lower; the oleyl amine of usining is simultaneously as reducing agent and solvent; triphenylphosphine is simultaneously as phosphorus source and protective agent; operating procedure is simple, reaction is gentleer; the pattern, the dimensional homogeneity that obtain product are good; semiconductor shell is the characteristics such as mono-crystalline structures, has overcome the deficiencies such as the required technique of prior art and system are complicated, crystal structure requirement is harsh, shell monocrystalline is bad.
The resulting Au/Ni of the present invention 12p 5the nanometer particle material of nucleocapsid structure has good stability and physicochemical properties, its excellent capacitive property, for it provides good basis in the electrochemical energy memory device applications of high-energy-density, high charge-discharge stability, can be widely used in the fields such as ultracapacitor, catalyst.
Accompanying drawing explanation
Fig. 1 is Au/Ni of the present invention 12p 5the nano particle preparation method's of nucleocapsid structure FB(flow block).
Fig. 2 is Au/Ni of the present invention 12p 5the XRD collection of illustrative plates of the nano particle of nucleocapsid structure
Fig. 3 is Au/Ni of the present invention 12p 5the EDX collection of illustrative plates of the nano particle of nucleocapsid structure.
Fig. 4 is Au/Ni of the present invention 12p 5the transmission electron microscope image of the nano particle of nucleocapsid structure
Fig. 5 is Au/Ni of the present invention 12p 5the high resolution electron microscope image of the nano particle of nucleocapsid structure.
Fig. 6 is Au/Ni of the present invention 12p 5the nano particle of nucleocapsid structure and pure Ni 12p 5and Au-Ni 12p 5polymer structure under different current densities than electric capacity comparative result.
Wherein, in Fig. 2,2 θ represent Bragg diffraction angle, symbol ● with ◆ mark respectively Au and Ni 12p 5the diffraction maximum position of component crystal face;
In Fig. 3, Au, Ni, P, C, O, Cu represent respectively gold, nickel, phosphorus, carbon, oxygen, copper;
Symbol █ in Fig. 6, ● from ▲ mark respectively pure Ni under different current densities 12p 5nano particle, Au/Ni 12p 5core-shell structure nanometer particle and Au-Ni 12p 5polymer structure nano particle is as the ratio electric capacity of electrode material for super capacitor.
The specific embodiment
The present invention synthesizes Au/Ni 12p 5the method of core-shell structure nanometer particle, is mainly to adopt converted in-situ in conjunction with the method for recrystallization, and the synthetic in advance Au-Ni dumbbell structure of take is presoma, adds triphenylphosphine, by Au-Ni dumbbell structure converted in-situ, is Au/Ni 12p 5nucleocapsid structure.The method comprises: as shown in Figure 1, and preparation Au nano particle, preparation Au-Ni dumbbell structure nano particle, converted in-situ, separation cleaning; Concrete steps are as follows:
(1), preparation Au nano particle: utilize the mixed solution of oleyl amine and nickel acetylacetonate as raw material, add chlorauric acid solution, obtain Au nano-particle solution after reaction;
(2), preparation Au-Ni dumbbell structure nano particle: the Au nano-particle solution that described step (1) is obtained heats up, and obtains Au-Ni dumbbell structure nanoparticles solution after reaction;
(3), converted in-situ: obtain in described Au-Ni dumbbell structure nanoparticles solution and add triphenylphosphine in step (2), after continuing to heat up, reaction obtains Au/Ni 12p 5the solution of core-shell structure nanometer particle;
(4), separation cleaning: by described Au/Ni 12p 5the separated Au/Ni that obtains of solution of core-shell structure nanometer particle 12p 5core-shell structure nanometer particle.
Method of the present invention, preferably, can adopt at 100 ℃ and nickel acetylacetonate is stirred in oleyl amine to dissolving, passes into afterwards the protective gas such as nitrogen or argon gas and splashes into gold chloride toluene solution and obtain Au nanoparticles solution; The Au nanoparticles solution of acquisition is warming up to 230 ℃ of oleyl amine reduction nickel acetylacetonates and obtains Au-Ni dumbbell structure; Add triphenylphosphine as phosphorus source and protective agent, be warming up to 270 ℃～320 ℃ original position conversion Au-Ni dumbbell structures and obtain Au/Ni 12p 5the solution of core-shell structure nanometer particle; Again to the Au/Ni making 12p 5the solution of core-shell structure nanometer particle carries out centrifugation, adds acetone to carry out ultrasonic cleaning precipitation, can obtain Au/Ni 12p 5core-shell structure nanometer particle.
The Au/Ni being prepared by said method 12p 5the characteristic that core-shell structure nanometer particle has is: this nano particle is face-centered cubic phase Au core and body-centered tetragonal phase Ni 12p 5shell forms, and wherein, golden nickle atom ratio is 8:92～15:85, described Au/Ni 12p 5the diameter of core-shell structure nanometer particle is at 15nm～30nm, and described Au nuclear diameter is 5nm～10nm; Wherein, the size of Au core and Ni 12p 5the thickness of shell increases along with adding the amount of gold chloride and nickel acetylacetonate mass penalty respectively.Described Ni 12p 5shell is mono-crystalline structures.
While also finding to adopt trioctyl phosphate to replace triphenylphosphine in the present invention, can not realize object of the present invention in the middle of research.
Below, further set forth the present invention with concrete preferred embodiment by reference to the accompanying drawings.Should be understood that these embodiment are only for the present invention is described, and be not used in restricted scope of the present invention.In following examples, the using method of unreceipted actual conditions is conventionally according to normal condition or the condition of advising according to manufacturer.
Embodiment 1
The present invention synthesizes Au/Ni 12p 5the method of the nano particle of nucleocapsid structure, preferably, the method includes the following step:
Step 1: 0.5g nickel acetylacetonate is added in 10ml oleyl amine, be warming up to 100 ℃ and mix to dissolving;
Step 2: the toluene solution of gold chloride (0.05g gold chloride is dissolved in 5ml toluene) is joined in the oleyl amine solution of step 1, pass into nitrogen (flow 60ml/min), at 100 ℃ of reaction 60min, the oleyl amine solution of the nickel acetylacetonate that obtains containing Au nano particle;
Step 3: the oleyl amine solution of step 2 is warming up to 230 ℃ of reaction 60min, utilizes oleyl amine reduction nickel acetylacetonate, obtain Au-Ni dumbbell structure nano particle;
Step 4: keep heating-up temperature constant, add 1g triphenylphosphine in the oleyl amine solution of step 3 acquisition Au-Ni dumbbell structure nano particle, be stirred to dissolving;
Step 5: make the first reactant liquor after adding the oleyl amine solution of triphenylphosphine to be warming up to 270 ℃ of reaction 60min step 4;
Step 6: the first reactant liquor that step 5 is made is cooled to after room temperature, centrifugal rotational speed is 10,000rpm～15, under 000rpm condition, centrifugation 10min obtains the first product;
Step 7: obtain the second product after the first product making in step 6 is utilized to 50ml acetone ultrasonic cleaning 5～10min in ultrasonic wave 50～100MHz;
Step 8: obtain third product after the second product making in step 7 is utilized to 50ml acetone ultrasonic cleaning 5～10min in ultrasonic wave 50～100MHz;
Step 9: the third product making in step 8 being utilized in ultrasonic wave 50～100MHz and obtain product after 50ml acetone ultrasonic cleaning 5～10min is the Au/Ni with monocrystalline shell 12p 5the nano particle of nucleocapsid structure.
The X ray diffracting spectrum of preparing product for said method as shown in Figures 2 and 3 with and power spectrum, determine that its composition and structure is face-centered cubic phase Au and body-centered tetragonal phase Ni 12p 5, golden nickle atom ratio is 8:92, nickel phosphorus atoms is than being 69:31.
The product of acquisition is carried out to transmission electron microscopy observation, transmission electron microscope image confirms that the product that as mentioned above prepared by method is nucleocapsid structure really, result as shown in Figure 4 and Figure 5, is the transmission electron microscope image under different amplification, shows the Au/Ni obtaining through above-mentioned synthetic method 12p 5the diameter of core-shell nano structure is at 16nm～20nm, and Au nuclear diameter is about 5nm; Semiconductor N i 12p 5shell is mono-crystalline structures; Between core and shell, do not determine crystal orientation.
The Au-Ni of comparative example 1 polymer structure 12p 5the preparation of composite nanoparticle
As a comparison case, the present invention prepares the Au-Ni of polymer structure 12p 5the method of composite nanoparticle, preferably, the method includes the following step:
Step 1: 0.5g nickel acetylacetonate is added in 10ml oleyl amine, be warming up to 100 ℃ and mix to dissolving;
Step 2: 1g triphenylphosphine is joined in the oleyl amine solution of step 1, pass into nitrogen (flow 60ml/min), stir 15min at 100 ℃;
Step 3: make the first reactant liquor after the oleyl amine solution of step 2 is warming up to 270 ℃ of reaction 60min;
Step 4: the first reactant liquor that step 3 is made is cooled to after room temperature, centrifugal rotational speed is that under 10000rpm～15000rpm condition, centrifugation 10min obtains the first product;
Step 5: obtain the second product after the first product making in step 4 is utilized to 50ml acetone ultrasonic cleaning 5～10min in ultrasonic wave 50～100MHz;
Step 6: obtain third product after the second product making in step 5 is utilized to 10ml chloroform ultrasonic cleaning 5～10min in ultrasonic wave 50～100MHz;
Step 7: obtain product for Ni after the third product making in step 6 being utilized in ultrasonic wave 50～100MHz to 10ml chloroform ultrasonic cleaning 5～10min 12p 5nano particle;
Step 8: the Ni that 0.44g step 7 is made 12p 5nano particle joins in 10ml oleyl amine, is warming up to 230 ℃ and mixes to dissolving;
Step 9: the toluene solution of gold chloride (0.05g gold chloride is dissolved in 5ml toluene) is joined in the oleyl amine solution of step 8, pass into nitrogen (flow 60ml/min), obtain the second reactant liquor at 230 ℃ of reaction 15min;
Step 10: the second reactant liquor that step 9 is made is cooled to after room temperature, centrifugal rotational speed is under 10000rpm～15000rpm condition, centrifugation 10min obtains the 4th product;
Step 11: obtain the 5th product after the 4th product making in step 10 is utilized to 50ml acetone ultrasonic cleaning 5～10min in ultrasonic wave 50～100MHz;
Step 12: obtain the 6th product after the 5th product making in step 11 is utilized to 50ml acetone ultrasonic cleaning 5～10min in ultrasonic wave 50～100MHz;
Step 13: obtain product for the Au-Ni of polymer structure after the 6th product making in step 12 is utilized to 50ml acetone ultrasonic cleaning 5～10min in ultrasonic wave 50～100MHz 12p 5nano particle.
The comparison of embodiment 2 capacitive properties
By the Au-Ni of the polymer structure of comparative example 1 preparation 12p 5the Au/Ni that composite nanoparticle and embodiment 1 are synthetic 12p 5the nano particle of nucleocapsid structure and pure Ni 12p 5the ratio capacitive property of nano particle under same test condition.Concrete test condition is: adopt three-electrode electro Chemical cell measuring system; By Au/Ni 12p 5core-shell structure nanometer particle and active carbon, polytetrafluoroethylene (PTFE) smear to 1cm after mixing with the mass ratio of 7:2:1 2nickel screen under 60 ℃ of vacuum, dry after as working electrode; Hg/HgO electrode and nickel screen are respectively as reference electrode with to electrode; The potassium hydroxide aqueous solution of 2mol/l of take is electrolyte.
Result as shown in Figure 6.Fig. 6 is under different current densities, the Ni of different component structures 12p 5the ratio capacitive property of based nano-material under same test condition.By contrasting us, can find to obtain Au/Ni by synthetic method of the present invention 12p 5the nano particle of nucleocapsid structure is than pure Ni 12p 5the Au-Ni of nano particle and polymer structure 12p 5composite nanoparticle has larger ratio electric capacity.Under the current density measuring condition of 0.2A/g, pure Ni 12p 5with Au/Ni 12p 5the ratio electric capacity of nucleocapsid structure is respectively 517.4 and 806.1F/g.Remove the quality of Au, the Au/Ni that synthetic method of the present invention obtains 12p 5core-shell nano structure, is compared and pure Ni up to 1007.8F/g than electric capacity 12p 5improve 94.7%.Result shows, the Au/Ni that synthetic method of the present invention obtains 12p 5the nano particle of nucleocapsid structure has excellent super capacitor performance.
With reference to embodiments of the invention, the present invention has been given to explanation above.But these embodiment are only used to illustrate object of the present invention, and are not intended to limit the scope of the invention, scope of the present invention is by claims and of equal value restriction thereof.Do not departing from the scope of the present invention, those skilled in the art can make multiple substituting and modification, and these substitute and revise and all should fall within the scope of the present invention.

Claims (10)

1. an Au/Ni 12p 5the nano particle of nucleocapsid structure, is characterized in that, this nano particle is face-centered cubic phase Au core and body-centered tetragonal phase Ni 12p 5shell forms, and wherein, golden nickle atom ratio is 8:92～15:85, described Au/Ni 12p 5the diameter of core-shell structure nanometer particle is at 15nm～30nm, and described Au nuclear diameter is 5nm～10nm; Described Ni 12p 5shell is mono-crystalline structures.
2. a synthetic Au/Ni 12p 5the method of the nano particle of nucleocapsid structure, is characterized in that, the method comprises:
(1), preparation Au nano particle: utilize the mixed solution of oleyl amine and nickel acetylacetonate as raw material, add chlorauric acid solution, obtain the oleyl amine solution containing the nickel acetylacetonate of Au nano particle after reaction;
(2), preparation Au-Ni dumbbell structure nano particle: the oleyl amine solution of the nickel acetylacetonate containing Au nano particle that described step (1) is obtained heats up, and obtains Au-Ni dumbbell structure nanoparticles solution after reaction;
(3), converted in-situ: obtain in described Au-Ni dumbbell structure nanoparticles solution and add triphenylphosphine in step (2), after continuing to heat up, reaction obtains Au/Ni 12p 5the solution of core-shell structure nanometer particle;
(4), separation cleaning: by described Au/Ni 12p 5the separated Au/Ni that obtains of solution of core-shell structure nanometer particle 12p 5core-shell structure nanometer particle.
3. method as claimed in claim 2; it is characterized in that; solvent at chlorauric acid solution described in step (1) is toluene; the reaction condition of described acquisition Au nano-particle solution is to be connected with under the condition of the protective gas such as nitrogen or argon gas; reaction temperature is 100 ℃, and the reaction time is at least 10min.
4. method as claimed in claim 2, is characterized in that, obtains the reaction condition of Au-Ni dumbbell structure nanoparticles solution for being 230 ℃ in temperature in described step (2), reacts at least 60min.
5. method as claimed in claim 2, is characterized in that, the reaction condition of converted in-situ described in described step (3), for being 270 ℃～320 ℃ in temperature, reacts at least 60min.
6. method as claimed in claim 2, is characterized in that, Au/Ni in described step (4) 12p 5the solution process centrifugation of core-shell structure nanometer particle, then pass through acetone ultrasonic cleaning, obtain the Au/Ni with monocrystalline shell 12p 5the nano particle of nucleocapsid structure.
7. method as claimed in claim 7, is characterized in that, the centrifuge speed of described centrifugation is 10000rpm～15000rpm, and centrifugation time is 10min.
8. method as claimed in claim 7, is characterized in that, the ultrasonic wave of described ultrasonic cleaning is 50MHz～100MHz, and wash number is at least 3 times.
9. by arbitrary described synthetic Au/Ni of method in claim 2-8 12p 5the nano particle of nucleocapsid structure, is characterized in that, described Au/Ni 12p 5the nano particle of nucleocapsid structure is face-centered cubic phase Au core and body-centered tetragonal phase Ni 12p 5shell forms, and wherein, golden nickle atom ratio is 8:92～15:85, described Au/Ni 12p 5the diameter of the nano particle of nucleocapsid structure is at 15nm～30nm, and described Au nuclear diameter is 5nm～10nm; Described Ni 12p 5shell is mono-crystalline structures.
10. the Au/Ni described in claim 1 or 9 12p 5the application of the nano particle of nucleocapsid structure in super capacitor material.
CN201410443538.XA 2014-09-02 2014-09-02 A kind of Au/Ni12p5nanoparticle of nucleocapsid structure and preparation method thereof Expired - Fee Related CN104190921B (en)

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