CN105148936B - Method for preparing straight-chain-arrangement cubical palladium-ferrum nanoparticles - Google Patents
Method for preparing straight-chain-arrangement cubical palladium-ferrum nanoparticles Download PDFInfo
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Abstract
The invention relates to a method for preparing straight-chain-arrangement cubical palladium-ferrum nanoparticles. The method comprises the following steps: (1) respectively dissolving 0.1-1.0 part (by mass) of CTAB (Cetyl Trimethyl Ammonium Bromide) and 1-5 parts (by mass) of glucose in 1-10 parts (by mass) of pure water and 10-50 parts (by mass) of pure water, so as to prepare a CTAB solution and a glucose solution; (2) respectively weighing 0.1-1 part (by mass) of the glucose solution prepared in the step (1) and 0.03-1 part (by mass) of the CTAB solution prepared in the step (1), adding the weighed glucose solution and the weighed CTAB solution into a beaker, and carrying out stirring, so as to form a uniform mixed solution; (3) adding 0.5-5.0 parts (by mass) of sodium tetrachloropalladate and 0.01-0.5 part (by mass) of ferric chloride into the mixed solution formed in the step (2), carrying out stirring until the solution is mixed uniformly, putting the mixture in a reaction kettle for hydrothermal reaction, heating the mixture to the temperature of 100-200 DEG C, and carrying out reaction for 0.5-5 hours; and (4) after the reaction ends, naturally cooling the reactant to room temperature, finally, pouring the reactant into a clean centrifuge tube, carrying out centrifuge washing for several times with anhydrous ethanol and ultrapure water, and baking obtained precipitates at the temperature of 25-80 DEG C, thereby obtaining a black powdered product. The product prepared by the method is regular in morphology, uniform in size, good in dispersity, high in electrocatalytic oxidation capacity, simple in preparation process and easy in condition control, so that scale production is facilitated.
Description
Technical field
The present invention relates to a kind of preparation method of palladium Fe nanometer particles, especially a kind of straight-chain arrangement cube palladium ferrum are received
The preparation method of rice corpuscles.
Technical background
Noble metal nano particles become inorganic because it has the ins and outs such as catalysis, plasma resonance, spectroscopy
One of widest system is studied in nano material.As nano material technology constantly develops and updates, pattern is studied（Size,
Shape etc.）Controllable nano material is widely paid close attention to by people.At present, large area, accurately control synthesis noble metal nano
Material, remains the focus and difficult point of current nano materials research.It is well known that using hydrothermal reduction method by your gold such as Pd, Au
Category reduction is a kind of typical Nobel-metal catalyst preparation method.
The content of the invention
To overcome above-mentioned the deficiencies in the prior art, it is an object of the invention to provide a kind of straight-chain arrangement cube palladium ferrum
The preparation method of nanoparticle, using surfactant cetyl trimethylammonium bromide（CTAB）, the week reduction of glucose
With Morphological control effect, under the synergism of CTAB and glucose, prepare with catenation, compound with regular structure, size
It is homogeneous, with good crystallinity and（100）The exposed cube nanometer Pd material of crystal face, improves the various property of precious metal material
Can, particularly greatly improve its catalytic performance.
For achieving the above object, present invention employs following technical scheme：
A kind of straight-chain arranges the preparation method of cube palladium Fe nanometer particles, and it comprises the steps：
1）By mass fraction, 0.1 ~ 1.0 part of CTAB and 1 ~ 5 part of glucose is dissolved in into respectively 1-10 parts and 10-50 parts are pure
In water, CTAB solution and glucose solution are made into.
2）By mass fraction, 0.1-1 part steps 1 are taken respectively）The glucose solution and 0.03-1 part steps 1 of gained）Gained
CTAB solution add jar agitation, form uniform mixed solution.
3）By mass fraction, by 0.5-5.0 part tetrachloro-palladium acid sodium（Na2PdCl4）With 0.01-0.5 part iron chloride（FeCl3）
It is added to step 2）Mixed solution in, until solution mix homogeneously, being put in reactor carries out hydro-thermal reaction, is warming up to for stirring
100 ~ 200 DEG C are reacted 0.5 ~ 5 hour.
4）After reaction terminates, room temperature is naturally cooled to.Reactant is finally poured into the centrifuge tube of cleaning, with dehydrated alcohol and
For several times, gained is deposited in 25-80 DEG C of drying and obtains black powder product ultra-pure water centrifuge washing.
The invention has the beneficial effects as follows：
1）The cube palladium ferrum nano material with the regular arrangement of one-dimensional straight-chain that the present invention is prepared, regular appearance,
Size uniformity, and favorable dispersibility.
2）Product prepared by the present invention has higher electrocatalytic oxidation ability.
3）The product preparation process of the present invention is simple, and condition is easily controllable, is easy to large-scale production.
Description of the drawings
Fig. 1 is the transmission electron microscope picture that the straight-chain of the present invention arranges cube palladium Fe nanometer particles.
Specific embodiment
To make purpose, technical scheme and the advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is
The a part of embodiment of the present invention, rather than the embodiment of whole.Based on the embodiment in the present invention, those of ordinary skill in the art
The every other embodiment obtained under the premise of creative work is not made, belongs to the scope of protection of the invention.
The present invention prepares out the cube palladium Fe nanometer particles with catenation by simple hydrothermal reduction method, improves
Electrocatalytic oxidation property.As shown in Figure 1.
A kind of straight-chain arranges the preparation method of cube palladium Fe nanometer particles, and it comprises the steps：
1）By mass fraction, 0.1 ~ 1.0 part of CTAB and 1 ~ 5 part of glucose is dissolved in into respectively 1-10 parts and 10-50 parts are pure
In water, CTAB solution and glucose solution are made into.
2）By mass fraction, 0.1-1 part steps 1 are taken respectively）The glucose solution and 0.03-1 part steps 1 of gained）Gained
CTAB solution add jar agitation, form uniform mixed solution.
3）By mass fraction, by 0.5-5.0 part tetrachloro-palladium acid sodium（Na2PdCl4）With 0.01-0.5 part iron chloride（FeCl3）
It is added to step 2）Mixed solution in, until solution mix homogeneously, being put in reactor carries out hydro-thermal reaction, is warming up to for stirring
100 ~ 200 DEG C are reacted 0.5 ~ 5 hour.
4）After reaction terminates, room temperature is naturally cooled to.Reactant is finally poured into the centrifuge tube of cleaning, with dehydrated alcohol and
For several times, gained is deposited in 25-80 DEG C of drying and obtains black powder product ultra-pure water centrifuge washing.
Embodiment 1：
A kind of straight-chain arranges the preparation method of cube palladium Fe nanometer particles, and it comprises the steps：
1）By mass fraction, during 0.1 part of CTAB and 1 part of glucose is dissolved in respectively into 1 part and 10 parts of pure water, CTAB is made into molten
Liquid and glucose solution.
2）By mass fraction, 0.1 part of step 1 is taken respectively）The glucose solution and 0.03 part of step 1 of gained）Gained
CTAB solution adds jar agitation, forms uniform mixed solution.
3）By mass fraction, by 0.5 part of tetrachloro-palladium acid sodium（Na2PdCl4）With 0.01 part of iron chloride（FeCl3）It is added to step
Rapid 2）Mixed solution in, until solution mix homogeneously, being put in reactor carries out hydro-thermal reaction for stirring, be warming up to 100 DEG C it is anti-
Answer 0.5 hour.
4）After reaction terminates, room temperature is naturally cooled to.Reactant is finally poured into the centrifuge tube of cleaning, with dehydrated alcohol and
For several times, gained is deposited in 25 DEG C of drying and obtains black powder product ultra-pure water centrifuge washing.
Embodiment 2：
A kind of straight-chain arranges the preparation method of cube palladium Fe nanometer particles, and it comprises the steps：
1）By mass fraction, during 0.5 part of CTAB and 3 part of glucose is dissolved in respectively into 5 parts and 30 parts of pure water, it is made into
CTAB solution and glucose solution.
2）By mass fraction, 0.5 part of step 1 is taken respectively）The glucose solution and 0.5 part of step 1 of gained）The CTAB of gained
Solution adds jar agitation, forms uniform mixed solution.
3）By mass fraction, by 3 parts of tetrachloro-palladium acid sodium（Na2PdCl4）With 0.3 part of iron chloride（FeCl3）It is added to step 2）
Mixed solution in, until solution mix homogeneously, being put in reactor carries out hydro-thermal reaction for stirring, is warming up to 150 DEG C of reactions 3
Hour.
4）After reaction terminates, room temperature is naturally cooled to.Reactant is finally poured into the centrifuge tube of cleaning, with dehydrated alcohol and
For several times, gained is deposited in 50 DEG C of drying and obtains black powder product ultra-pure water centrifuge washing.
Embodiment 3：
A kind of straight-chain arranges the preparation method of cube palladium Fe nanometer particles, and it comprises the steps：
1）By mass fraction, during 1.0 parts of CTAB and 5 part of glucoses are dissolved in respectively into 10 parts and 50 parts of pure water, it is made into
CTAB solution and glucose solution.
2）By mass fraction, 1 part of step 1 is taken respectively）The glucose solution and 1 part of step 1 of gained）The CTAB solution of gained
Jar agitation is added, uniform mixed solution is formed.
3）By mass fraction, by 5.0 parts of tetrachloro-palladium acid sodium（Na2PdCl4）With 0.5 part of iron chloride（FeCl3）It is added to step
2）Mixed solution in, until solution mix homogeneously, being put in reactor carries out hydro-thermal reaction, is warming up to 200 DEG C of reactions for stirring
5 hours.
4）After reaction terminates, room temperature is naturally cooled to.Reactant is finally poured into the centrifuge tube of cleaning, with dehydrated alcohol and
For several times, gained is deposited in 80 DEG C of drying and obtains black powder product ultra-pure water centrifuge washing.
Claims (1)
1. a kind of straight-chain arranges the preparation method of cube palladium Fe nanometer particles, it is characterised in that it comprises the steps：
1) by mass fraction, 0.1~1.0 part of CTAB and 1~5 part of glucose is dissolved in respectively in 1-10 parts and 10-50 part pure water,
It is made into CTAB solution and glucose solution；
2) by mass fraction, 0.1-1 part steps 1 are taken respectively) obtained by glucose solution and 0.03-1 part steps 1) obtained by
CTAB solution adds jar agitation, forms uniform mixed solution；
3) by mass fraction, by 0.5-5.0 part tetrachloro-palladium acid sodium (Na2PdCl4) and 0.01-0.5 part iron chloride (FeCl3) add
To step 2) mixed solution in, until solution mix homogeneously, being put in reactor carries out hydro-thermal reaction, is warming up to 100 for stirring
~200 DEG C are reacted 0.5~5 hour；
4) after reaction terminates, room temperature is naturally cooled to；
5) finally by step 4) products therefrom be poured into cleaning centrifuge tube, with dehydrated alcohol and ultra-pure water centrifuge washing for several times, institute
25-80 DEG C of drying must be deposited in and obtain black powder product.
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| CN201510449935.2A CN105148936B (en) | 2015-07-29 | 2015-07-29 | Method for preparing straight-chain-arrangement cubical palladium-ferrum nanoparticles |
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| CN102989450B (en) * | 2012-12-03 | 2015-03-11 | 中国科学院大连化学物理研究所 | Preparation method, structural feature and application of carrying type nanometer electrocatalyst |
| CN104174392B (en) * | 2013-05-27 | 2016-08-10 | 中国科学院大连化学物理研究所 | One one step preparation method of a kind of loaded platino multimetal reforming catalyst and application |
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