CN106670495A - Preparation method of network-state Ag-Au-Pd trimetal porous material - Google Patents
Preparation method of network-state Ag-Au-Pd trimetal porous material Download PDFInfo
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- CN106670495A CN106670495A CN201510759603.4A CN201510759603A CN106670495A CN 106670495 A CN106670495 A CN 106670495A CN 201510759603 A CN201510759603 A CN 201510759603A CN 106670495 A CN106670495 A CN 106670495A
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- deionized water
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/52—Gold
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
Abstract
The invention provides a preparation method of a network-state Ag-Au-Pd trimetal porous material. Under proper conditions, the surface of a spongy silver nano structure suspending in a mixed solution of chloroauric acid and potassium chloropalladate is subjected to fast and partial replacement; and generated gold nano particles and palladium nano particles are uniformly distributed, and a rough surface is formed. By changing the concentration of the mixed solution, surface roughness and the metal atom ratio can be effectively adjusted and controlled. Under the circumstance that the total content of noble metals, namely Au and Pd, is quite low, in other words, the sum of the atomic percentages is lower than 10%, the Ag-Au-Pd trimetal porous material shows ultrahigh SERS detection flexibility for rhodamine B molecules adsorbed to the surface of the Ag-Au-Pd trimetal porous material and has quite high catalytic activity for a sodium borohydride reduction 4-nitrophenol reaction system. The preparation method is quick, low in cost and easy to apply on a large-scale; and an effective path is provided for preparing a multi-metal porous nano material.
Description
Technical field
The present invention relates to a kind of metal porous materials of network-like Ag-Au-Pd tri- with the sensitivity of superelevation SERS Yu superelevation catalysis activity
The preparation method of material, especially, displacement of the method based on inexpensive, easy prepare with scale is reacted, and reaction condition is gentle, weight
Renaturation is good, and is easily controlled.
Background technology
Noble metal (Au Ag Pt Pd) nano material due in catalysis, bio-sensing, optics and Molecular Detection (such as
SERS (SERS)) etc. field there is wide application prospect and of great interest.Its performance is depended primarily on
The pattern and size (such as pore size) of material.Metal nanoparticle shows high chemical reactivity because of dimensional effect,
But they are easy to there is aggregation and is difficult to reuse.Apparent yardstick be submicron order, with three-dimensional netted nano-pore structure
Material is not only avoided that these shortcomings of nano-particle, and possesses more reactivity regions.Especially, its three-D pore structure
More SERS " focus " and catalytic active site can be provided in third dimension.
Many metal nano materials combine the interfacial effect of electro transfer between cooperative effect and metal between metal, and particularly, performance can
Regulated and controled by ratio between metal.A large amount of researchs with regard to bimetal nanostructure material both at home and abroad show, specific surface area, gold
The raising to catalysis activity such as category interface has conclusive effect.However, many with regard to the metals of network-like Ag-Au-Pd tri- at present
The research of hole nano material is still rarely reported.
The present invention proposes a kind of preparation method of the metal polyporous materials of network-like Ag-Au-Pd tri-.Under proper condition, it is suspended in
There is quick, aliquot replacement, the gold of generation, palladium in the sponge silver nanostructured surface in gold chloride, potassium chloropalladate mixed solution
Nano-particle is uniformly distributed and is formed rough surface.In the case where noble metal Au and Pd total contents are very low, (atomic percent is low
In 10%), rhodamine B molecule displays of the metal polyporous materials of Ag-Au-Pd tri- for absorption on its surface go out the SERS of superelevation
Detection sensitivity, has very high catalysis activity to sodium borohydride reduction 4- nitrophenols reaction system.
The content of the invention
The purpose of the present invention：A kind of preparation method of the metal polyporous materials of network-like Ag-Au-Pd tri- is proposed, and introduces it in SERS
The application of Molecular Detection and catalytic field.The preparation method low cost, reaction is gentle (only needing heating water bath).By same
When control the concentration of gold chloride and potassium chloropalladate, regulate and control the surface roughness and bi-metal interface of product, it is achieved thereby that superelevation
SERS sensitivity and high catalytic activity.The preparation method will have good application prospect in the preparation field of multifunctional porous material.
The technical scheme is that：Certain density sodium borohydride and silver nitrate solution are prepared, 25mL sodium borohydrides is taken water-soluble
Liquid, adds 5mL glycerine；In the case where room temperature is stirred vigorously, 5mL silver nitrate solutiones are rapidly joined, question response is after 5 minutes,
Suspension is filtered and deionized water cleaning, freeze-drying 6-10 hours obtain sponge silver nanostructured；Then, by 3-10
The sponge silver nanostructured that mg is dried is added in the mixed solution being made up of 1-4mL gold chlorides and potassium chloropalladate, and solvent is
The mixed liquor of deionized water and ethylene glycol, with vigorous stirring, after reacting 10 minutes under 50-70 DEG C of constant temperature, by suspension
Take out, be put into saturated aqueous common salt and soak, then deionized water is cleaned repeatedly, finally product is put into baking oven and is dried.
When preparing sponge silver nanostructured, sodium borohydride is respectively 0.05-0.2M with the optimum concentration range of silver nitrate aqueous solution
And 0.02-0.04M.
25mL sodium borohydride solutions are taken, 5mL glycerine is added, in the case where room temperature is stirred vigorously, 5mL silver nitrates is rapidly joined
Solution, question response filtered suspension and deionized water cleaning after 5 minutes, and freeze-drying 6-10 hours obtain sponge silver
Nanostructured.
Solution and sponge silver nanostructured can be configured under conditions of room temperature or slightly above room temperature.
Displacement reaction is prepared during the metal polyporous materials of network-like Ag-Au-Pd tri-, and dry sponge silver nanostructured takes 3-10
Mg, in being added to the mixed solution being made up of 1-4mL gold chlorides and potassium chloropalladate, solvent is the mixed of deionized water and ethylene glycol
Liquid is closed, both volume ratios are 1: 10～1: 5.
In mixed solution, gold chloride concentration range is 11.58 × 10-7M～20.58 × 10-7M, potassium chloropalladate concentration range is
2.57×10-7M～11.58 × 10-7M。
With vigorous stirring, after reacting 10 minutes under 50-70 DEG C of constant temperature.
Reacted product needs to be put into saturated aqueous common salt and soaks, so as to remove the AgCl accessory substances of Surface Creation.
Compared with other methods, the sponge silver nanostructured that the first step of the present invention is synthesized by wet chemistry method, without the need for any addition
Agent or template；Second step displacement reaction only need to be carried out under lower temperature (50-70 DEG C), and duration 10min is obtained
The metal polyporous materials of network-like Ag-Au-Pd tri-.Preparation method proposed by the present invention is quick, low cost, be easy to scale.
Beneficial effects of the present invention：
(1) propose it is a kind of prepare it is metal porous with the network-like Ag-Au-Pd tri- of high catalytic activity with SERS hypersensitivitys
The method of material, is successfully obtained using line replacement reaction is entered under 60 DEG C of heating water baths.
(2) compared with other methods, the preparation method also has following particular advantages：
1. any additive and template, simple to operate, quick, low cost are not needed in preparation process；
2. controllability is good, by adjusting the controllable Product size of gold chloride and potassium chloropalladate concentration and metallic atom ratio；
3. it is with low cost, with good industrial applications prospect；
4. strong applicability, extends to other multifunctional nano porous materials.
Description of the drawings
Fig. 1 is the XRD diffraction patterns of (a) spongy Nano Silver and Ag-Au-Pd；(b) spongy Nano Silver and (c) three metal
The FESEM figures of nanostructured, illustration is the picture before and after single silver-colored connecting line displacement reaction.
Fig. 2 is the EDX and Surface scan figure (illustration) of the network-like metal polyporous materials of Ag-Au-Pd tri- of different component shown in Fig. 1.(a)
Ag91.8Au4.5Pd3.7；(b)Ag91.3Au5.5Pd3.2；(c)Ag90Au7.8Pd2.2；(d)Ag89.1Au9.1Pd1.8；(e)Ag88.9Au9.4Pd1.7。
Fig. 3 is (a) sponge silver nanostructured；(b)Ag91.8Au4.5Pd3.7；(c)Ag90Au7.8Pd2.2；(d)Ag89.1Au9.1Pd1.8；
(e)Ag88.9Au9.4Pd1.7For the 10 of adsorption-6The SERS spectra figure of M rhodamine B molecules.
Fig. 4 is color change of (a) 4-NP solution before and after catalytic reaction；In the network-like Ag of 0.5mg (b)90Au7.8Pd2.2Receive
Under rice structure and (c) sponge silver nanostructured catalyst, the ultraviolet-visible absorption spectroscopy of sodium borohydride reduction 4-NP solution is inserted
Figure is reaction rate.
Fig. 5 be (a) different component Ag-Au-Pd porous materials 400nm in 4-NP catalytic reactions at absorbance logarithm with react when
Between graph of a relation；The graph of a relation of (b) gold/palladium atomic ratio and reaction rate.
Specific embodiment
The present invention is reacted using displacement and be successfully obtained the metal polyporous materials of network-like Ag-Au-Pd tri-, and specific embodiment is as follows：
Embodiment 1
The preparation of the metal polyporous materials of network-like Ag-Au-Pd tri-：Sponge silver nanostructured is prepared first：Configuration concentration is 0.1
The NaBH of M4The mixed solution (5mL glycerine mixes with 25mL deionized waters) of water/glycerine, is stirred vigorously in room temperature
Under, by the AgNO that 5mL concentration is 0.025M3The aqueous solution is rapidly joined, and persistently stirring treats that solution becomes clarification.Use deionization
Water cleans black suspension thing, then freeze-drying 6 hours.Then, the sponge silver nanostructured that 5mg is dried is added to
In the mixed solution be made up of 2mL gold chlorides and potassium chloropalladate, solvent is mixed liquor (both volumes of deionized water and ethylene glycol
Than for 1: 8), gold chloride concentration is 11.58 × 10-7M, potassium chloropalladate concentration is 11.58 × 10-7M.With vigorous stirring, 60 DEG C
After reacting 10 minutes under constant temperature, suspension is taken out, be put into saturated aqueous common salt and soak, then deionized water is cleaned repeatedly,
Finally product is put into baking oven and is dried at 50 DEG C.
Fig. 1 (a) is XRD peak value of the sponge silver nanostructured of the acquisition of embodiment 1 before displacement reaction occurs and after generation
Comparison diagram.Can find that the peak width of 4 crystal faces has after catalytic reaction generation substantially to broaden, and the peak value of (200) crystal face is to (111)
The peak value ratio of crystal face declines.Fig. 1 (b) and (c) respectively replace the SEM figures before and after reaction, it can be seen that porous is received
Rice structure does not have significant change.However, finding out from the TEM figures of illustration, constitute cancellated nano silver wire surface and occur in that
The particle of diameter about 5nm.Fig. 2 (a) is the EDS collection of illustrative plates of the products therefrom of embodiment 1, and element Surface scan figure shows in illustration,
Gold, palladium element are evenly coated at the surface of porous silver.Can draw, metallic atom ratio is Ag: Au: Pd=91.8: 4.5: 3.7.
Therefore, the sample is named as Ag91.8Au4.5Pd3.7。
Embodiment 2
It is 13.89 × 10 to change gold chloride concentration-7M, potassium chloropalladate concentration is 9.26 × 10-7M, other conditions and the phase of embodiment 1
Together.
Fig. 2 (b) is the EDS collection of illustrative plates of the products therefrom of embodiment 2.Can draw, metallic atom is Ag: Au: Pd=91.3: 5.5: 3.2.
Therefore, the sample is named as Ag91.3Au5.5Pd3.2。
Embodiment 3
It is 18.52 × 10 to change gold chloride concentration-7M, potassium chloropalladate concentration is 4.63 × 10-7M, other conditions and the phase of embodiment 1
Together.
Fig. 2 (c) is the EDS collection of illustrative plates of the products therefrom of embodiment 3.Can draw, metallic atom ratio is Ag: Au: Pd=
91.3∶7.8∶2.2.Therefore, the sample is named as Ag90Au7.8Pd2.2。
Embodiment 4
It is 19.84 × 10 to change gold chloride concentration-7M, potassium chloropalladate concentration is 3.31 × 10-7M, other conditions and the phase of embodiment 1
Together.
Fig. 2 (d) is the EDS collection of illustrative plates of the products therefrom of embodiment 4.Can draw, metallic atom ratio is Ag: Au: Pd=
89.1∶9.1∶1.8.Therefore, the sample is named as Ag89.1Au9.1Pd1.8。
Embodiment 5
It is 20.58 × 10-7M to change gold chloride concentration, and potassium chloropalladate concentration is 2.57 × 10-7M, other conditions and embodiment 1
It is identical.
Fig. 2 (e) is the EDS collection of illustrative plates of the products therefrom of embodiment 5.Can draw, metallic atom ratio is Ag: Au: Pd=
89.1∶9.4∶1.7.Therefore, the sample is named as Ag88.9Au9.4Pd1.7。
Embodiment 6
When SERS Molecular Detection sample preparations are carried out to sample, the nano material for taking 2.0mg dryings is placed on slide, then by 50
Microlitres 10-6M rhodamine Bs solution is added dropwise, and dries in atmosphere.Fig. 3 is that sponge silver nanostructured and different component are network-like
The metal polyporous materials of Ag-Au-Pd tri- are directed to the 10 of adsorption-6The SERS detection spectrograms of M rhodamine B molecules.Can see
Go out, rhodamine B molecule displays of the metal polyporous materials of all of Ag-Au-Pd tri- for absorption on its surface go out the SERS of superelevation
Detection sensitivity, performance is superior to sponge silver nanostructured (curve a).Particularly, sample Ag89.1Au9.1Pd1.8SERS
Detection sensitivity preferably (curve d).
Embodiment 7
When testing the catalytic performance of sample, the sodium borohydride solution for taking 0.2mL 0.1M is added to 2.8mL 4 × 10-5M
4- nitro phenol solutions in, then 0.5mg catalyst is added and ultra-violet absorption spectrum test is carried out immediately.Seen by Fig. 4 (a)
Observe, the network-like Ag of addition 0.5mg90Au7.8Pd2.2Afterwards, 4- nitros phenol solution faded quickly in 3.5 minutes, showed 4-
Nitrophenols has been completely reduced.The maximum of 4- nitrophenols solution absorption peaks is absorbed at wavelength 400nm by 400nm
Absorption intensity continues to increase at the lasting reduction of intensity and 295nm, it is known that 4- nitrophenols is 4- amino by sodium borohydride reduction
Phenol, illustration is catalytic rate.Fig. 4 (b) is the UV, visible light of sodium borohydride reduction 4- nitro phenol solutions in catalytic reaction process
Absorption spectrum.Can be drawn by illustration linear relationship chart, catalytic rate is 1.23 × 10-2/s.Its catalytic rate is apparently higher than in phase
With spongy silver nanostructured catalytic rate (as illustrated in fig. 4 c) under test condition.
Fig. 5 (a) be different component Ag-Au-Pd porous materials at 400nm in 4-NP catalytic reactions absorbance logarithm with it is anti-
Answer time chart, it can be seen that network-like Ag90Au7.8Pd2.2The catalysis activity highest of nanostructured.This performance optimization knot
Fruit is consistent with the conclusion of Au/Pd atomic ratio alternation relation curves with reaction rate constant in Fig. 5 (b).
Claims (7)
1. a kind of preparation method of the metal polyporous materials of network-like Ag-Au-Pd tri-, is characterized in that, prepare certain density sodium borohydride and silver nitrate solution, take 25mL sodium borohydride aqueous solutions, add 5mL glycerine；In the case where room temperature is stirred vigorously, 5mL silver nitrate solutiones are rapidly joined, question response filtered suspension and deionized water cleaning after 5 minutes, and freeze-drying 6-10 hours obtain sponge silver nanostructured；Then, the sponge silver nanostructured that 3-10mg is dried is added in the mixed solution being made up of 1-4mL gold chlorides and potassium chloropalladate, solvent is the mixed liquor of deionized water and ethylene glycol, with vigorous stirring, after reacting 10 minutes under 50-70 DEG C of constant temperature, suspension is taken out, be put into saturated aqueous common salt and soak, again deionized water is cleaned repeatedly, finally product is put into baking oven and is dried.
2. preparation method according to claim 1, it is characterised in that when preparing sponge silver nanostructured, sodium borohydride is respectively 0.05-0.2M and 0.02-0.04M with the concentration of silver nitrate aqueous solution.
3. preparation method according to claim 1, it is characterized in that, take 25mL sodium borohydride solutions, add 5mL glycerine, in the case where room temperature is stirred vigorously, 5mL silver nitrate solutiones are rapidly joined, question response is after 5 minutes, suspension is filtered and deionized water cleaning, freeze-drying 6-10 hours obtain sponge silver nanostructured.
4. preparation method according to claim 1, it is characterised in that aliquot replacement reaction is carried out by sponge silver nanostructured and gold chloride, potassium chloropalladate mixed solution and prepares the metal polyporous materials of network-like Ag-Au-Pd tri-.
5. the preparation method of the metal polyporous materials of network-like Ag-Au-Pd tri- according to claim 1, it is characterized in that, the sponge silver nanostructured that 3-10mg is dried is added in the mixed solution being made up of 1-4mL gold chlorides and potassium chloropalladate, wherein, gold chloride concentration range is 11.58 × 10-7M～20.58 × 10-7M, potassium chloropalladate concentration range is 2.57 × 10-7M～11.58 × 10-7M。
6. preparation method according to claim 1, it is characterised in that for deionized water and the mixed liquor of ethylene glycol, both volume ratios are 1: 10～1: 5 to the solvent that configuration gold chloride is adopted with potassium chloropalladate mixed solution.
7. preparation method according to claim 1, it is characterised in that with vigorous stirring, after reacting 10 minutes under 50-70 DEG C of constant temperature, suspension is taken out, be put into saturated aqueous common salt and soak, again deionized water is cleaned repeatedly, finally product is put into baking oven and is dried.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108195832A (en) * | 2018-01-19 | 2018-06-22 | 东南大学 | The method and detection kit of abio-arsenic residues in a kind of detection water |
| CN108971512A (en) * | 2018-09-14 | 2018-12-11 | 江西科技师范大学 | A kind of the green preparation and its application of the rectangular particle of porous spongy Ag |
| CN110767913A (en) * | 2019-11-07 | 2020-02-07 | 安徽师范大学 | Single silver-palladium alloy nanowire electrode and preparation method and application thereof |
| CN112404448A (en) * | 2019-08-23 | 2021-02-26 | 南京智融纳米新材料科技有限公司 | Low-temperature large-scale preparation method of three-dimensional reticular nano-structure metal foam material |
| CN115636942A (en) * | 2022-09-21 | 2023-01-24 | 华东理工大学 | Preparation method of high-spin Fe3+ trimetal MIL-101 (FeNiTi) material |
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| CN115636942A (en) * | 2022-09-21 | 2023-01-24 | 华东理工大学 | Preparation method of high-spin Fe3+ trimetal MIL-101 (FeNiTi) material |
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Application publication date: 20170517 |