WO2012012927A1 - Procédés pour la synthèse de nanofils ultrafins de métal noble en phase aqueuse et l'organisation de films nanoporeux de métal noble par auto-sédimentation. - Google Patents

Procédés pour la synthèse de nanofils ultrafins de métal noble en phase aqueuse et l'organisation de films nanoporeux de métal noble par auto-sédimentation. Download PDF

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WO2012012927A1
WO2012012927A1 PCT/CN2010/002238 CN2010002238W WO2012012927A1 WO 2012012927 A1 WO2012012927 A1 WO 2012012927A1 CN 2010002238 W CN2010002238 W CN 2010002238W WO 2012012927 A1 WO2012012927 A1 WO 2012012927A1
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nanowires
noble metal
metal
mixture
synthesized
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PCT/CN2010/002238
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English (en)
Chinese (zh)
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刘景富
刘睿
于素娟
江桂斌
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中国科学院生态环境研究中心
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Publication of WO2012012927A1 publication Critical patent/WO2012012927A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
    • 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
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0547—Nanofibres or nanotubes

Definitions

  • the invention relates to a method for constructing a precious metal nanoporous membrane by supercritical nanowire aqueous phase synthesis and ultrafine metal nanowire self-sedimentation, and particularly relates to a method suitable for the construction of nanowires and nanoporous membranes in the field of catalysis. Background technique
  • the use of stabilizers that bind weakly to nanomaterials can also increase the activity of nanocatalysts when synthesizing nanocatalysts.
  • strong binding of stabilizers or polymers can effectively improve the stability of the catalyst, it has been reported that the catalytic activity of uncoated nano-gold particles in glucose oxidation is as high as 18043 moles of gluconic acid per mole of gold per hour, and surfactant-depleted palladium is removed.
  • the activity of nanoparticles in electrocatalytic oxidation of formic acid is much higher than that of commercial palladium/carbon catalysts. It is still a problem to synthesize nanocatalysts with high activity and high stability.
  • nanoporous materials metal parts and voids between several nanometers and tens of nanometers
  • nanoporous materials have both nanoscale microstructures and microscale macrostructures. Therefore, nanoporous materials have a large specific surface area, a higher atomic ratio of unsaturated atoms, and better stability. These advantages make this nanoporous material an excellent catalyst/electrocatalyst, sensor and energy conversion building unit.
  • the means for obtaining such nanostructures are chemical/electrochemical corrosion alloys, metallization of non-metallic nanoporous structures, and self-assembly of stencil-controlled nanoparticles.
  • Methods for synthesizing precious metal nanowires which have been reported in the literature include a hard stencil method and a soft stencil method.
  • the former uses mesoporous silicon or carbon nanotubes as a hard template to limit/inducing the growth of nanowires, or to have nanometers with reducibility Lines (such as selenium nanowires) as sacrificial templates; the latter include micelles/reverse micelles, DNA or bacteria) stenciling, and directional bonding under the control of amines (oleylamine, octadecylamine, hexadecylamine) (Oriented Attachment) 0
  • these synthetic methods require the use of organic solvents, strongly bound stabilizers/ligands, and higher synthesis temperatures have been aged for extended periods of time.
  • the object of the present invention is to provide a method for synthesizing precious metal ultrafine nanowires in an aqueous phase, which can synthesize ultrafine nanowires of metal, such as gold, palladium, platinum and the like, which have application prospects in the aqueous phase, and the synthesis cost Low cost, one hundred milligrams of nanowires can be synthesized at one time, and the synthesized nanowires have high activity in electrocatalytic oxidation of methanol/ethanol.
  • Another object of the present invention is to provide a method for constructing a precious metal nanoporous material (nanoporous film), which can obtain a nanoporous film having a thickness of several tens of nanometers to several micrometers by self-precipitation of the corresponding precious metal ultrafine nanowires.
  • the obtained nanoporous membrane has a large specific surface area and a metal fraction size of less than 5 nm, and is expected to be used in catalytic and analytical chemical related fields such as surface enhanced Raman spectroscopy (SERS) and surface assisted laser desorption ionization mass spectrometry (SADLI-MS). ).
  • the present inventors have completed the present invention through intensive research.
  • a method of synthesizing precious metal ultrafine nanowires comprising the steps of:
  • step (e) centrifuging the mixture obtained in step (d) at a temperature of 50-70 ° C, and separating the mixture into a supernatant liquid and a two-phase system containing the lower cloud point phase of the nano material;
  • the stirring speed is 1000 rpm.
  • the centrifugation temperature is 50 °C.
  • the agitation time in step (b) is 5 minutes.
  • the precious metal precursor has a concentration of 1 mmol'I
  • the ratio is 0.05 ° /.
  • the amount of (w/v) is the nonionic surfactant added in the step (a).
  • the reducing agent used is potassium borohydride or sodium borohydride.
  • nonionic surfactant is selected from the group consisting of
  • Triton TX-114 Triton TX-100.
  • the synthetic environment is an ice bath.
  • the synthesized nanowires are ultrafine, networked, and polycrystalline nanowires of 3 nanometers or less.
  • the method has the following advantages: 1. Wide applicability: It can synthesize three different metal nanowires such as Au, Pd and Pt; 2. Greenness of the method: It is not necessary to use chemicals that are toxic (such as chloroform), odor (amines), expensive or not yet commercialized (Triton TX-114 has good biocompatibility);
  • the method can be carried out in normal temperature or ice bath, and only takes a few minutes, and does not need to react for several tens of hours in high temperature;
  • This method is based on the very weak interaction between the benzene ring and the precious metal on TX-114 to control the morphology, which is beneficial to the retention of active sites.
  • the method uses cloud point extraction as a separation stabilization method, and the nanowires can be preserved for a long time (several weeks) because there is no corrosion effect of Cr.
  • a method for constructing a precious metal nanoporous membrane comprising the steps of:
  • the concentration of ethanol used therein is 50% (V/V).
  • the method has the following advantages:
  • the method is based on the very weak interaction between the benzene ring and the precious metal on the TX-114. It is very easy to clean and has a simple ethanol cleaning.
  • the metal content can be as high as 94% (EDS, energy scattering spectrometry);
  • the method obtains a controllable thickness of the nanopore film, and by changing the depth of the solution, obtaining a nanopore film thickness of several tens of nanometers to several micrometers;
  • the constructed nanoporous membrane has a large specific surface and a low relative density, such as a gold nanoporous membrane with a specific surface area of up to 14.7 m 2 /g and a relative density as low as 7.5%.
  • FIG. 1 is a corresponding transmission electron micrograph (left image) and size distribution (right panel) of the synthesis of the gold ultrafine nanowire of Example 1.
  • Fig. 2 is a corresponding transmission electron micrograph (left image) and size distribution (right image) of the Pt ultrafine nanowires synthesized in Example 2.
  • Fig. 3 is a corresponding transmission electron micrograph (left image) and size distribution (right image) of the Pd ultrafine nanowires synthesized in Example 3.
  • Figure 4 is a high resolution scanning electron micrograph (left) of the gold nanopore film constructed on a silicon wafer in Example 4 and the corresponding solution depth/nanoporous film thickness relationship (right).
  • Fig. 5 is a view showing the construction of a palladium nanopore film on the basis of a silicon wafer in Example 6.
  • Fig. 6 is a view showing the construction of a platinum nanopore film on the basis of a silicon wafer in Example 7.
  • the nanostructure morphology can be controlled by controlling the concentration ratio of the reducing agent to the metal precursor in the presence of a suitable nonionic surfactant, when the concentration ratio is At 1 o'clock, only the nanoparticles are formed. As the concentration of the reducing agent increases, the proportion and length of the nanowires in the product increase simultaneously. Finally, when the concentration ratio reaches 6, 4 and 2, respectively, the obtained product is completely gold nanowires, platinum nanowires. And palladium nanowires. Further research found that TX-114 is weakly bonded to the surface of nanomaterials through the benzene ring, and this combination has a choice.
  • a method of synthesizing precious metal ultrafine nanowires comprising the steps of:
  • the nonionic surfactant is selected from the group consisting of Triton TX-114 (polyoxyethylene (8) nonylphenyl ether, available from Acros Oganic, USA), Triton TX-100 ( Polyoxyethylene (10) octylphenyl ether, available from Acros Oganic, Inc., USA, preferably Triton TX-114, preferably at a concentration of 0.05% (w/v).
  • the metal precursor is HAuCl 4 , H 2 PtCl 6 and Pd(N0 3 ) 2o
  • the present invention also provides a method for constructing a precious metal nanoporous membrane, the method comprising the steps of: (a) placing the cleaned substrate (silicon wafer, ITO slide, optical slide, etc.) on the bottom of the flat-bottomed container and adding the synthetic precious metal nanowires to the desired depth;
  • the nonionic surfactant is selected from the group consisting of Triton TX-114 (polyoxyethylene (8) nonylphenyl ether, available from Acros Oganic, USA), Triton TX-100 ( Polyoxyethylene (10) octylphenyl ether, available from Acros Oganic, Inc., USA, preferably Triton TX-114, preferably at a concentration of 0.05% (w/v).
  • Triton TX-114 polyoxyethylene (8) nonylphenyl ether, available from Acros Oganic, USA
  • Triton TX-100 Polyoxyethylene (10) octylphenyl ether, available from Acros Oganic, Inc., USA, preferably Triton TX-114, preferably at a concentration of 0.05% (w/v).
  • the metal precursors are HAuCl 4 , 3 ⁇ 4 ⁇ 03 ⁇ 4 and Pd(N0 3 ) 2 .
  • the C1-salt is a water-soluble salt of a Group I element or a Group II element, such as NaCl, LiCK KCK CaCl 2 , MgCl 2 , etc., wherein NaCl is preferred.
  • the C1-salt is used in an amount of from 0.01 to 1% by weight, preferably 0.2% by weight, based on the weight percent of the mixture obtained in the step (b).
  • the C1-salt is NaCl or KC1.
  • Triton TX-114 (available from Acros Oganic, USA);
  • Triton TX-100 (available from Acros Oganic, USA);
  • HAuC, H 2 PtCl 6 was purchased from Sinopharm Chemical Reagent Co., Ltd.;
  • Pd(N0 3 ) 2 was purchased from Xitou Chemical Plant, Shantou, Guangdong;
  • the water used is Millipore ultrapure water (18.2 ⁇ )
  • TX-114 as a stabilizer and structure control agent, and KB as a reducing agent.
  • 0.05 mmol of HAuCl 4 and 25 mg of TX-114 were dissolved in 47 ml of Millipore ultrapure water, and then added to a sealed 50 ml Erlenmeyer flask. After stirring for 5 minutes at 1000 rpm in an ice bath, 3 ml of 100 mM KBH 4 solution was quickly injected into the solution with a syringe. Continue stirring for 10 seconds, the color of the solution changes from bright yellow to brown, and the red finally turns dark gray.
  • TX-114 as a stabilizer and structure control agent, and KB as a reducing agent.
  • 0.05 mmol H 2 PtCl 6 and 25 mg TX-114 were dissolved in 48 ml of Millipore ultrapure water, and then added to a sealed 50 ml Erlenmeyer flask. After stirring for 5 minutes at 1000 rpm in an ice bath, 2 ml of 100 mM KBH was quickly injected into the solution with a syringe. 4 solution, continue to stir for 10 seconds. After the reaction was completed, 25 mg of TX-114 was added to the solution, and the mixture was homogenized.
  • TX-114 is used as a stabilizer and structure control agent, and KBH 4 is a reducing agent.
  • 0.05 mmol of Pd(N0 3 ) 2 and 25 mg of TX-114 were dissolved in 49 ml of Millipore ultrapure water, and then added to a sealed 50 ml Erlenmeyer flask. After stirring for 5 minutes at 1000 rpm in an ice bath, a lml was quickly injected into the solution with a syringe. 100 mM BH 4 solution, stirring was continued for 10 seconds. After the reaction was completed, 25 mg of TX-114 was added to the solution and mixed uniformly at 60.
  • Example 4 Constructing a gold nanopore film on a silicon wafer basis
  • the ultrafine gold nanowires were synthesized as described in Example 1.
  • the lcm x lcm silicon wafer which had been ultrasonically cleaned with hydrochloric acid, ethanol and ultrapure water was placed at the bottom of the crystallizing dish, and the synthesized gold nanowire solution was added to the depth.
  • 0.5cm, lcm, 2cm, 3cm and 4cm (because it is added to the inside of the crystallizing dish, the height of the solution can be measured), and it is allowed to stand at 4 °C for 12 hours.
  • the upper gray-brown solution becomes colorless, and the upper layer is discarded.
  • the supernatant is dried by drying the lower gel at 40% relative humidity, and after washing with ethanol, a gold nanopore film is obtained.
  • the gold nanopore film was synthesized as described in Example 4, and the substrate was changed from a silicon wafer to a bismuth glass.
  • the obtained gold nanopore film was subjected to cyclic voltammetry in 0.1 M HC10 4 , and the specific surface area of the gold nanopore film was 15.6 m 2 /g as measured by the amount of reduction of gold.
  • Example 6 Based on silicon wafer Construction of palladium nanoporous membrane
  • the ultrafine palladium nanowires were synthesized as described in Example 2, and NaCl was added to a concentration of 6 mM, and the mixture was stirred and mixed.
  • the lcm x lcm silicon wafer which had been ultrasonically cleaned with hydrochloric acid, ethanol and ultrapure water was placed at the bottom of the crystallizing dish.
  • Example 7 Construction of a platinum nanoporous film based on a silicon wafer
  • the ultrafine platinum nanowires were synthesized as described in Example 2.
  • the lcm x lcm silicon wafer which had been ultrasonically cleaned by using hydrochloric acid, ethanol and ultrapure water was placed at the bottom of the crystallizing dish, and the above synthesized platinum nanowire solution/dispersion was added.
  • the upper solution becomes colorless, discard the supernatant, the lower gel is dried at 40% relative humidity, and after washing with ethanol, platinum nanopores can be obtained.
  • membrane A Top-view scanning electron microscope (SEM S-3000, S-4800, Hitachi) observed that the nanoporous film consisted of platinum nanowires with a diameter of about 2.5 nm and pores of about 5-20 nm (see Figure 6).

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Catalysts (AREA)

Abstract

L'invention porte sur des procédés pour la synthèse de nanofils de métal noble (Au, Pd, Pt) et l'organisation de films nanoporeux de métal noble par auto-sédimentation. Les procédés comprennent les étapes suivantes : le tensioactif non ionique à hauteur de 0,05% (w/v) est ajouté à la solution de précurseur de métal noble (HAuCl4, H2PtCl6, Pd(NO3)2) ayant une concentration de 1 mmol-l-1 qui est ensuite agitée et mélangée. Du KBH4 (ou NaBH4) est ajouté à hauteur de 6 fois, 4 fois et 2 fois la quantité du précurseur de métal pour HAuCl4, H2PtCl6, et Pd (NO3)2 respectivement, après que le mélange a été agité pendant 5-10 minutes dans une solution aqueuse glacée. Le précurseur de métal présent dans le mélange est complètement réduit pour synthétiser lesdits nanofils métalliques ultrafins (≤ 3 nm) enchevêtrés sous agitation vigoureuse. Par l'ajout supplémentaire du tensioactif non ionique à hauteur de 0,05 % (w/v) dans la solution de dispersion de nanofils synthétisés, le mélange uniformément et la centrifugation à 60°C pendant 10 minutes, le matériau de dimension nanométrique peut être séparé et purifié. Les films nanoporeux de métal noble correspondants peuvent être formés par l'ajout de NaCl jusqu'à 5 mM (l'ajout supplémentaire de NaCl n'est pas nécessaire pour le nanofil d'Au) dans la solution de dispersion aqueuse de nanofils synthétisés et le fait de laisser la solution reposer pendant 12 heures.
PCT/CN2010/002238 2010-07-29 2010-12-31 Procédés pour la synthèse de nanofils ultrafins de métal noble en phase aqueuse et l'organisation de films nanoporeux de métal noble par auto-sédimentation. WO2012012927A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN2010102398195A CN101935017B (zh) 2010-07-29 2010-07-29 用于贵重金属超细纳米线水相合成及其自沉降构建贵重金属纳孔膜的方法
CN201010239819.5 2010-07-29

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CN102826527B (zh) * 2012-08-21 2014-07-09 西北大学 一种稀土掺杂的Ca-PO4-CO3固溶超细纳米线的制备方法
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