CN105032412A - Silver/platinum alloy nanometer material with porous hollow structure and preparing method thereof - Google Patents
Silver/platinum alloy nanometer material with porous hollow structure and preparing method thereof Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention belongs to the field of function materials and relates to a silver/platinum alloy nanometer material with a porous hollow structure and a preparing method thereof. The component of the silver/platinum alloy nanometer material with the porous hollow structure is the alloy of Ag and Pt, the particle size is 5 nm to 40 nm, the hollow inner diameter is 1 nm to 25 nm, and the silver/platinum alloy nanometer material with the porous hollow structure is in a popcorn shape. The preparing method comprises 1) preparing sodium citrate solution, adding inorganic silver salt precursor, mixing the sodium citrate solution and the inorganic silver salt precursor to obtain mixed liquor, and adding sodium borohydride to mix continuously to obtain silver seed crystal solution; and 2) adding inorganic platinum slat, polyvinylpyrrolidone and ascorbic acid into the silver seed crystal solution prepared from the step 1) and cooling, centrifuging and taking sedimentation after heating reaction to obtain the sliver/platinum nanometer material with the porous hollow structure. The preparing method is simple in technology, simple and convenient to operate, high in repeatability, mild in reaction condition and environmentally friendly. The prepared silver/platinum alloy nanometer material with the porous hollow structure has the advantages of having high superficial area, high electrocatalytic activity, high stability and low cost.
Description
Technical field
The invention belongs to field of functional materials, silver/platinum alloy nano material specifically relating to a kind of porous hollow structure and preparation method thereof.
Background technology
Fuel cell is a kind of electrochemical appliance, and it is without hot merit conversion process, but is directly electric energy by chemical energy by electrochemical means.And heat engine is that heat energy carrys out work done again and is converted into electric energy, so the utilization ratio of energy is lower than fuel cell system by reacting the chemical energy that discharges.Such as, with H
2the efficiency of internal combustion engine for fuel is 10% ~ 20%, and same with H
2fuel cell efficiency for fuel then can reach 45% ~ 50% (theoretical value is 93%), and therefore the research boom of fuel cell rises in worldwide.It take fuel cell as the automobile (ToyotaFCV) of power that the Toyota Company of recent Japan has issued what within 2015, will go on the market, also imply that fuel cell will move towards civilian market, has market potential and application prospect.
One of critical material of fuel cell is the eelctro-catalyst that electrode uses, for the electrochemical reaction of catalytic fuel or oxidant.Current extensive use be the catalyst that is active material with platinum (Pt), as platinum C catalyst (Pt/C), but platinum based catalyst is expensive, causes the totle drilling cost of fuel cell to remain high.In order to reduce the cost of fuel cell, the research direction of current fuel-cell catalyst is mainly divided into platinum based catalyst and non-platinum catalyst, wherein platinum based catalyst is divided into three major types again: (1) pure platinum catalyst, and mainly through regulating and controlling the pattern of platinum grain, crystal face improves performance; (2) platinum alloy catalyst, make alloy to improve performance mainly through being mixed by platinum in other metals, wherein platinum alloy catalyst is subject to extensive concern, and the Science paper that M.Markovic delivered 2007 time finds Pt
3the electro catalytic activity of Ni alloy material is far above Pt monocrystal material, the research of Pt alloy catalyst subsequently obtains more development, as the patent (Chinese patent CN201210041267) etc. preparing hollow Platinum alloy material with hydro-thermal method of Shandong University's application; (3) platinum/metallic catalyst, preparation example, as the heterodimer of nucleocapsid structure, utilizes the intermetallic performance being used for improving catalyst.But not the catalyst of platinum then has By Non-precious Metal Catalysts, palladium-based catalyst, transition metal macrocyclic compound derivative and non-metallic catalyst.
Summary of the invention
The problems such as the cost that the object of the invention is to exist for existing fuel cell is high, efficiency is low, poor performance, life-span are short, provide silver/platinum alloy nano material of a kind of porous hollow structure that cost is low, efficiency is high, performance is good, the life-span is long and preparation method thereof.
The component of the silver/platinum alloy nano material of described porous hollow structure is the alloy of Ag and Pt, and particle diameter is 5 ~ 40nm, and hollow internal diameter is 1 ~ 25nm, flower-shaped in rice krispies.
The preparation method of the silver/platinum alloy nano material of described porous hollow structure, comprises the following steps:
1) prepare sodium citrate solution, add inorganic silver salt precursor body, obtain mixed liquor after stirring, then add sodium borohydride, continue to stir, obtain silver-colored seed-solution;
2) in step 1) add inorganic platinum salt, polyvinylpyrrolidone (K=30) and ascorbic acid in obtained silver-colored seed-solution, after adding thermal response, cooling centrifuging and taking precipitation, obtains the silver/platinum alloy nano material of porous hollow structure.
In step 1) in, the molar concentration of described sodium citrate solution can be 0.0010 ~ 0.5000M; Described inorganic silver salt precursor body can be 1 with the ratio of the amount of substance of natrium citricum in solution: (1 ~ 4); Described sodium borohydride can be (3 ~ 1) with the thing mass ratio of the inorganic silver salt precursor body added: 1; Described inorganic silver salt precursor body can be selected from the one in silver carbonate, silver nitrate, silver sulfate etc.; The time of described stirring can be 6 ~ 48h.
In step 2) in, described inorganic platinum salt and step 1) described in the thing mass ratio of inorganic silver salt precursor body can be 1: (0.1 ~ 10); Described inorganic platinum salt can be selected from the one in chloroplatinic acid, potassium hexachloroplatinate, potassium tetrachloroplatinate, platinum nitrate etc.; Described inorganic platinum salt, thing mass ratio between polyvinylpyrrolidone (K=30) and ascorbic acid can be 40: 1: 300; The described temperature adding thermal response can be 60 ~ 100 DEG C, and the time adding thermal response can be 30 ~ 240min.
The present invention adopts platinum and the low silver of cost to form metal alloy, and decrease the consumption of platinum, cost is lower than the material of pure platinum; And hollow porous structure has very large surface area, ensure that the performances such as the catalysis of material; Silver/platinum alloy then has stronger resistance to the catalyst poisoning of CO; So preparation method's technique provided by the present invention is simple, easy and simple to handle, repeatability is high, the reaction condition of use is gentle, environmentally friendly; Silver/platinum alloy the nano material of prepared porous hollow structure has the advantages such as high surface, high electrocatalytic active, high stability and low cost, pure platinum can be replaced as the catalyst in fuel cell membrane electrode, greatly reduce the cost of fuel cell.In addition, the silver/platinum alloy nano material of prepared porous hollow structure also has potential using value in chemical sensor, chemical catalysis and photocatalysis field.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of the silver/platinum alloy nano material of embodiment 1 porous hollow structure.Scale is 0.2 μm.
Fig. 2 is the transmission electron microscope picture of the silver/platinum alloy nano material of embodiment 1 porous hollow structure.Scale is 100nm.
Fig. 3 is the XRD figure of the silver/platinum alloy nano material of embodiment 1 porous hollow structure.Abscissa is two times of incident angles (2-Theta, 2 θ), and ordinate is diffracted intensity (Intensity).
Fig. 4 is the transmission electron microscope picture of the silver/platinum alloy nano material of embodiment 2 porous hollow structure.In the diagram, the scale of a is the scale of 100nm, b is 20nm.
Fig. 5 is the transmission electron microscope picture of the silver/platinum alloy nano material of embodiment 2 porous hollow structure.Scale is 5nm.
Fig. 6 is the element distribution analysis result of the silver/platinum alloy nano material of embodiment 2 porous hollow structure.
Detailed description of the invention
Following examples will the present invention is further illustrated by reference to the accompanying drawings.
Embodiment 1
Get 0.0285g natrium citricum and 0.0180g silver nitrate, be dissolved in 30mL deionized water, be placed in flask stirred at ambient temperature; What in reactant liquor, then add 0.6mL newly joins the sodium borohydride solution that concentration is 0.1M, and now solution changes black into by water white transparency, then becomes brown color, obtains silver-colored seed-solution after Keep agitation 6h, takes out, under being stored in the environment of 4 DEG C.
0.0372g potassium platinic chloride is added in the silver-colored seed-solution preparing gained, 0.0800g ascorbic acid, 0.0510g polyvinylpyrrolidone (K=30), stirs and is heated to 80 DEG C, and reactant liquor is become after black from brown color and remains on 80 DEG C of stirrings, reaction bulb is taken off after 0.5h, reactant liquor is transferred in centrifuge tube, rotates 60min with the speed of 11000rpm, after centrifugal, remove supernatant, leave precipitation, obtain the silver/platinum alloy nano material of porous hollow structure.
Fig. 1 provides the transmission electron microscope picture of the silver/platinum alloy nano material of embodiment 1 porous hollow structure, and photo display nano particle is porous air heart shaped, and size is homogeneous, favorable dispersibility; Fig. 2 provides the transmission electron microscope picture of the silver/platinum alloy nano material of embodiment 1 porous hollow structure, and the size of photo display particle mostly is 5 ~ 40nm; Fig. 3 provides the XRD figure of the silver/platinum alloy nano material of embodiment 1 porous hollow structure, and the peak in the face, (111)/(200) of Ag and Pt is very close, overlaps.Embodiment 2
Get 0.0143g natrium citricum and 0.0050g silver carbonate, be dissolved in 20mL deionized water, be placed in flask stirred at ambient temperature; What in reactant liquor, then add 0.3mL newly joins the sodium borohydride solution that concentration is 0.1M, and now solution changes black into by water white transparency, then becomes brown color, obtains silver-colored seed-solution after Keep agitation 24h, takes out, under being stored in the environment of 4 DEG C.
0.0060g Platinous Potassium Chloride, 0.0160g ascorbic acid and 0.0180g polyvinylpyrrolidone (K=30) is added in the silver-colored seed-solution preparing gained, stir while be heated to 70 DEG C, reactant liquor is become after black from brown color and remains on 90 DEG C of stirrings, reaction bulb is taken off after 2h, reactant liquor is transferred in centrifuge tube, rotates 60min with the speed of 11000rpm, after centrifugal, remove supernatant, leave precipitation, obtain the silver/platinum alloy nano material of porous hollow structure.
Fig. 4 provides the transmission electron microscope picture of the silver/platinum alloy nano material of embodiment 2 porous hollow structure; Picture display material becomes porous air heart shaped, and size is homogeneous, is of a size of 5 ~ 40nm; Fig. 5 provides the transmission electron microscope picture of the silver/platinum alloy nano material of embodiment 2 porous hollow structure, and particle has good lattice fringe, means to have good crystal structure; Fig. 6 provides the element distribution analysis result of the silver/platinum alloy nano material of embodiment 2 porous hollow structure, display be the distribution of Ag and Pt, the signal of photo display Ag and the Pt of both superpositions overlaps mutually, and both explanations exist with alloy form.
Embodiment 3
Be the sodium citrate solution of 0.5000M with natrium citricum and deionized water compound concentration, get 100mL in flask, add the silver sulfate of 3.8975g, at the uniform velocity stir under room temperature, then slowly drip 5mL and dissolved 1.3875gNaBH
4deionized water, solution becomes black from water white transparency, becomes brown color subsequently, obtains silver-colored seed-solution after Keep agitation 48h, take out, under being stored in the environment of 4 DEG C.
12.9250g chloroplatinic acid, 33.0000g ascorbic acid and 0.1800g polyvinylpyrrolidone (K=30) is added in the silver-colored seed-solution preparing gained, stir while be heated to 60 DEG C, reactant liquor is become after black from brown color and remains on 90 DEG C of stirrings, reaction bulb is taken off after 4h, reactant liquor is transferred in centrifuge tube, 60min is rotated with the speed of 11000rpm, supernatant is removed after centrifugal, leave precipitation, obtain the silver/platinum alloy nano material of porous hollow structure, effect is with embodiment 1.
Embodiment 4
Be the sodium citrate solution of 0.0050M with natrium citricum and deionized water compound concentration, get 20mL in flask, add the silver nitrate of 0.017g, at the uniform velocity stir under room temperature, then slowly drip 5mL and dissolved 0.0038gNaBH
4deionized water, solution becomes black from water white transparency, becomes light yellow subsequently, obtains silver-colored seed-solution after Keep agitation 36h, take out, under being stored in the environment of 4 DEG C.
0.0447g Platinous Potassium Chloride, 0.1320g ascorbic acid and 0.0090g polyvinylpyrrolidone (K=30) is added in the silver-colored seed-solution preparing gained, stir while be heated to 70 DEG C, reactant liquor from light yellow become black after remain on 100 DEG C of stirrings, reaction bulb is taken off after 1h, reactant liquor is transferred in centrifuge tube, 60min is rotated with the speed of 11000rpm, supernatant is removed after centrifugal, leave precipitation, obtain the silver/platinum alloy nano material of porous hollow structure, effect is with embodiment 2.
Embodiment 5
By the method identical with embodiment 1, be 48h unlike the mixing time when preparing silver-colored crystal seed, effect is with embodiment 1.Embodiment 6
By the method identical with embodiment 1, unlike the use of inorganic platinum salt be chloroplatinic acid, final effect is with embodiment 1.Embodiment 7
By the method identical with embodiment 2, unlike remaining on 70 DEG C of stirrings after adding inorganic platinum salt always, reaction bulb is taken off after 2h, 60min is rotated with the speed of 11000rpm, supernatant is removed after centrifugal, leave precipitation, obtain the silver/platinum alloy nano material of porous hollow structure, effect is with embodiment 2.
Embodiment 8
By the method identical with embodiment 3, unlike remaining on 80 DEG C of stirrings after adding inorganic platinum salt, reaction bulb is taken off after 0.5h, 60min is rotated with the speed of 11000rpm, supernatant is removed after centrifugal, leave precipitation, obtain the silver/platinum alloy nano material of porous hollow structure, effect is with embodiment 1.
Embodiment 9
By the method identical with embodiment 4, the sodium citrate solution concentration unlike preparation is 0.0010M, and the amount of taking is 100mL.After adding inorganic platinum salt, remain on 80 DEG C of stirrings, take off reaction bulb after 4h, rotate 60min with the speed of 11000rpm, remove supernatant after centrifugal, leave precipitation, obtain the silver/platinum alloy nano material of porous hollow structure, effect is with embodiment 1.
Claims (10)
1. silver/platinum alloy nano material of porous hollow structure, it is characterized in that its component is the alloy of Ag and Pt, particle diameter is 5 ~ 40nm, and hollow internal diameter is 1 ~ 25nm, flower-shaped in rice krispies.
2. the preparation method of the silver/platinum alloy nano material of porous hollow structure as claimed in claim 1, is characterized in that comprising the following steps:
1) prepare sodium citrate solution, add inorganic silver salt precursor body, obtain mixed liquor after stirring, then add sodium borohydride, continue to stir, obtain silver-colored seed-solution;
2) in step 1) add inorganic platinum salt, polyvinylpyrrolidone and ascorbic acid in obtained silver-colored seed-solution, after adding thermal response, cooling centrifuging and taking precipitation, obtains the silver/platinum alloy nano material of porous hollow structure.
3. the preparation method of the silver/platinum alloy nano material of porous hollow structure as claimed in claim 2, is characterized in that in step 1) in, the molar concentration of described sodium citrate solution is 0.0010 ~ 0.5000M.
4. the preparation method of the silver/platinum alloy nano material of porous hollow structure as claimed in claim 2, is characterized in that in step 1) in, described inorganic silver salt precursor body is 1 with the ratio of the amount of substance of natrium citricum in solution: (1 ~ 4); Described sodium borohydride can be (3 ~ 1) with the thing mass ratio of the inorganic silver salt precursor body added: 1.
5. the preparation method of the silver/platinum alloy nano material of porous hollow structure as claimed in claim 2, is characterized in that in step 1) in, described inorganic silver salt precursor body is selected from the one in silver carbonate, silver nitrate, silver sulfate.
6. the preparation method of the silver/platinum alloy nano material of porous hollow structure as claimed in claim 2, is characterized in that in step 1) in, the time of described stirring is 6 ~ 48h.
7. the preparation method of the silver/platinum alloy nano material of porous hollow structure as claimed in claim 2, it is characterized in that in step 2) in, described inorganic platinum salt and step 1) described in the thing mass ratio of inorganic silver salt precursor body be 1: (0.1 ~ 10).
8. the preparation method of the silver/platinum alloy nano material of porous hollow structure as claimed in claim 2, is characterized in that in step 2) in, described inorganic platinum salt is selected from the one in chloroplatinic acid, potassium hexachloroplatinate, potassium tetrachloroplatinate, platinum nitrate.
9. the preparation method of the silver/platinum alloy nano material of porous hollow structure as claimed in claim 2, is characterized in that in step 2) in, described inorganic platinum salt, thing mass ratio between polyvinylpyrrolidone and ascorbic acid are 40: 1: 300.
10. the preparation method of the silver/platinum alloy nano material of porous hollow structure as claimed in claim 2, is characterized in that in step 2) in, described in add thermal response temperature be 60 ~ 100 DEG C, the time adding thermal response is 30 ~ 240min.
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Cited By (10)
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| CN105537612A (en) * | 2015-12-15 | 2016-05-04 | 安徽工业大学 | Micro-structure porous sliver and preparation method thereof |
| CN105702972A (en) * | 2016-04-12 | 2016-06-22 | 燕山大学 | Cathode catalyst for fuel cell and preparation method of cathode catalyst |
| CN105771979A (en) * | 2016-03-22 | 2016-07-20 | 安徽师范大学 | Platinum/silver alloy nano-particle catalyst, method for preparing same and application of platinum/silver alloy nano-particle catalyst |
| CN105776131A (en) * | 2016-04-21 | 2016-07-20 | 厦门大学 | Silver platinum nanocomposite loaded on graphene surface and preparation method thereof |
| CN107275649A (en) * | 2017-05-27 | 2017-10-20 | 陕西师范大学 | A kind of preparation method of platinum-silver alloys hollow Nano flower |
| CN110093777A (en) * | 2019-05-23 | 2019-08-06 | 余晨 | A kind of industrialized process for preparing of conductive fiber |
| CN110216295A (en) * | 2019-07-08 | 2019-09-10 | 鲁东大学 | A kind of the room temperature aqueous phase preparation method and its glucose electrocatalytic oxidation of silver nano flower-like |
| CN110433841A (en) * | 2019-07-22 | 2019-11-12 | 盐城工学院 | A kind of preparation method containing nitrogen vacancy azotized carbon nano piece composite photo-catalyst of Ag-Pt bimetallic load |
| CN112687902A (en) * | 2020-12-28 | 2021-04-20 | 龙岩学院 | Preparation method of nitrogen-doped graphene-supported hollow nano platinum composite material |
| CN113319288A (en) * | 2021-04-28 | 2021-08-31 | 南京师范大学 | Preparation method and application of hollow Pt four-footed nano material |
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| CN105537612A (en) * | 2015-12-15 | 2016-05-04 | 安徽工业大学 | Micro-structure porous sliver and preparation method thereof |
| CN105537612B (en) * | 2015-12-15 | 2017-07-18 | 安徽工业大学 | A kind of porous silver of micro-structural and preparation method thereof |
| CN105771979A (en) * | 2016-03-22 | 2016-07-20 | 安徽师范大学 | Platinum/silver alloy nano-particle catalyst, method for preparing same and application of platinum/silver alloy nano-particle catalyst |
| CN105702972A (en) * | 2016-04-12 | 2016-06-22 | 燕山大学 | Cathode catalyst for fuel cell and preparation method of cathode catalyst |
| CN105776131A (en) * | 2016-04-21 | 2016-07-20 | 厦门大学 | Silver platinum nanocomposite loaded on graphene surface and preparation method thereof |
| CN107275649B (en) * | 2017-05-27 | 2020-04-24 | 陕西师范大学 | Preparation method of platinum-silver alloy hollow nanoflower |
| CN107275649A (en) * | 2017-05-27 | 2017-10-20 | 陕西师范大学 | A kind of preparation method of platinum-silver alloys hollow Nano flower |
| CN110093777A (en) * | 2019-05-23 | 2019-08-06 | 余晨 | A kind of industrialized process for preparing of conductive fiber |
| CN110216295A (en) * | 2019-07-08 | 2019-09-10 | 鲁东大学 | A kind of the room temperature aqueous phase preparation method and its glucose electrocatalytic oxidation of silver nano flower-like |
| CN110433841A (en) * | 2019-07-22 | 2019-11-12 | 盐城工学院 | A kind of preparation method containing nitrogen vacancy azotized carbon nano piece composite photo-catalyst of Ag-Pt bimetallic load |
| CN110433841B (en) * | 2019-07-22 | 2022-01-25 | 盐城工学院 | Preparation method of Ag-Pt bimetallic supported carbon nitride nanosheet composite photocatalyst containing nitrogen vacancies |
| CN112687902A (en) * | 2020-12-28 | 2021-04-20 | 龙岩学院 | Preparation method of nitrogen-doped graphene-supported hollow nano platinum composite material |
| CN112687902B (en) * | 2020-12-28 | 2022-06-10 | 龙岩学院 | Preparation method of nitrogen-doped graphene-supported hollow nano platinum composite material |
| CN113319288A (en) * | 2021-04-28 | 2021-08-31 | 南京师范大学 | Preparation method and application of hollow Pt four-footed nano material |
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