CN1424149A - Method for coating mono-metal particles on carbon nano tube surface - Google Patents
Method for coating mono-metal particles on carbon nano tube surface Download PDFInfo
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- CN1424149A CN1424149A CN 02160191 CN02160191A CN1424149A CN 1424149 A CN1424149 A CN 1424149A CN 02160191 CN02160191 CN 02160191 CN 02160191 A CN02160191 A CN 02160191A CN 1424149 A CN1424149 A CN 1424149A
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Abstract
A process for carrying the nano metal particles on the surface of carbon nanotube features that said metal may be Pt, Pd, Ru, Au and Ag, and includes such steps as uniformly and proportionally dispersing the carbon nanotubes in the solution of metal salt in polyol and heating by microwave radiation. Its advantages are small diameter of metal particle (3-4 nanos), high speed, and high efficiency.
Description
Technical field
The present invention relates to the preparation of nano metal particles, relate in particular to a kind of method at carbon nano tube surface loaded with nano monometallic nano particle.
Background technology
Carbon nanometer tube has excellent physics and chemical property with its particular structure, has utilization widely.The nano tubular structure of CNT makes it become a kind of new catalyst carrier, for example has good catalytic performance in carbon nano tube surface supporting Pt and metallic such as grade.By mixed acid carbon nano tube surface is carried out oxidation processes, can improve metal in its surperficial load behavior with nitric acid or sulfuric acid-nitric acid.What but carrying method in the past still adopted is general immersion-reduction technique, just at first the carbon nanometer tube after handling is immersed in the solution that contains slaine, make slaine be adsorbed on the surface (the interior pipe that enters carbon nanometer tube is also arranged) of carbon nanometer tube, make its high temperature reduction under reducing atmosphere then.The method that also can adopt vapour deposition and chemical plating in addition is in carbon nano tube surface burden metal nanoparticle or nanometer film.But these methods are difficult to the size of control load at the metallic particles of carbon nano tube surface, and it distributes also than broad.For example document [1] report adopt immersion-reduction technique in the average grain diameter of the particle of Pd, Pt, Ag and the Au of carbon nano tube surface load respectively 7,8,17,8nm, particle size distribution is at 2-12nm.And the performance of catalyst is subjected to metal nanoparticle size and inhomogeneity significant impact, and general particle diameter is more little even more, and its catalytic performance is good more.Therefore carbon nano tube surface how load have and littler have practice with the more uniform nano metal particles of size and be worth.
Add hot reflux by the polyhydric alcohol solutions that contains slaine, at high temperature polyalcohol is used at carbon nano tube surface loaded with nano metal particle this polyol process of solution metal ion reduction formation nano particle as reducing agent.Its typical process is to add hot reflux to contain the ethylene glycol solution of precious metal salt and the mixture of CNT, and at high temperature ethylene glycol makes metal ion reduction as reducing agent and loads on the surface of CNT.But this traditional hot reflux that adds needs 1-3h, also is not easy to control the size of final nano particle.
Document [1] Xue B, Chen P, Hong Q, Lin JY, Tan KL, Growth of Pd, Pt, Ag and Aunanoparticles on carbon nanotubes, JOURNAL OF MATERIALS CHEMISTRY11 (9): 2378-2381 2001.
Summary of the invention
The purpose of this invention is to provide a kind of method at carbon nanometer tube area load nanometer monometallic particle.
It is that even carbon nanotube is dispersed in a kind of polyhydric alcohol solutions of slaine, adopts the homogeneous mixture of this CNT of carry out microwave radiation heating and slaine polyhydric alcohol solutions then.The polyhydric alcohol solutions of per 1 liter slaine contains 0.2～8 gram CNT; The concentration of slaine is 0.0002～0.03 mol in the slaine polyhydric alcohol solutions.
Advantage of the present invention is that the platinum-ruthenium alloy nano particle diameter in the carbon nano tube surface load is tiny, and average grain diameter is in 3～4 nanometers, and has narrow grain through Size Distribution.Metallic is 5%～42% in the load capacity of carbon nano tube surface.The present invention also has fast, and is simple, the advantage that efficient is high.The metal nanoparticles loaded material of this carbon nanometer tube has utilization widely in electrochemical energy conversion and catalytic field.
The specific embodiment
Above-mentioned slaine is: chloroplatinic acid, potassium chloroplatinate, platinum acetate, ruthenic chloride, gold chloride, silver nitrate, palladium bichloride, palladium; Polyalcohol is an ethylene glycol; CNT is multi-walled carbon nano-tubes or SWCN.
Embodiment 1:
Many walls carbon nanometer tube of 0.08 gram is dispersed in 50 milliliters the ethylene glycol solution that contains 0.0001 mole of chloroplatinic acid uniformly, and heating is 1 minute under 700 watts microwave radiation.The average grain diameter of the nanometer platinum particles of transmission electron microscope observing carbon nanometer tube area load is at 3.5nm, and grain is through being distributed between the 2-4nm.Platinum nanoparticles is 19% in the load capacity of carbon nano tube surface.And with the average grain diameter of the nanometer platinum particles of the carbon nanometer tube load of traditional immersion-method of reducing preparation at 7.6nm, grain is through being distributed between the 2-11nm.
Embodiment 2:
The single wall carbon nanometer tube of 0.01 gram is dispersed in 50 milliliters the ethylene glycol solution that contains 0.00001 molar acetate platinum uniformly, heating is 1 minute under 700 watts microwave radiation. and the average grain diameter of the nanometer platinum particles of transmission electron microscope observing carbon nanometer tube area load is at 3.3nm, grain is through being distributed between the 2-4nm, and platinum nanoparticles is 16% in the load capacity of carbon nano tube surface.And with the average grain diameter of the nanometer platinum particles of the carbon nanometer tube load of traditional immersion-method of reducing preparation at 6.6nm, grain is through being distributed between the 1-9nm.
Embodiment 3:
Many walls carbon nanometer tube of 0.4 gram is dispersed in 50 milliliters the ethylene glycol solution that contains 0.0015 mole of potassium chloroplatinate uniformly, heating is 1 minute under 700 watts microwave radiation. and the average grain diameter of the nanometer platinum particles of transmission electron microscope observing carbon nanometer tube area load is at 3.6nm, grain is through being distributed between the 2-4nm, and platinum nanoparticles is 42% in the load capacity of carbon nano tube surface.And with the average grain diameter of the nanometer platinum particles of the carbon nanometer tube load of traditional immersion-method of reducing preparation at 7.8nm, grain is through being distributed between the 1-13nm.
Embodiment 4:
Many walls carbon nanometer tube of 0.02 gram is dispersed in 50 milliliters the ethylene glycol solution that contains 0.00005 mole of ruthenic chloride uniformly, and heating is 1 minute under 700 watts microwave radiation.The average grain diameter of the nanometer ruthenium particle of transmission electron microscope observing carbon nanometer tube area load is at 3.2nm, and grain is through being distributed between the 2-4nm, and the ruthenium metal nanoparticle is 20% in the load capacity of carbon nano tube surface.And with the average grain diameter of the nanometer platinum particles of the carbon nanometer tube load of traditional immersion-method of reducing preparation at 6.1nm, grain is through being distributed between the 1-9nm.
Embodiment 5:
Many walls carbon nanometer tube of 0.09 gram is dispersed in 50 milliliters the ethylene glycol solution that contains 0.00005 molar acetate palladium uniformly, and heating is 1 minute under 700 watts microwave radiation.The average grain diameter of the nanometer cake particle of transmission electron microscope observing carbon nanometer tube area load is at 3.8nm, and grain is through being distributed between the 2-4.2nm, and metal nanoparticle is 5.5% in the load capacity of carbon nano tube surface.And with the average grain diameter of the nanometer platinum particles of the carbon nanometer tube load of traditional immersion-method of reducing preparation at 6.8nm, grain is through being distributed between the 1-12.3nm.
Embodiment 6:
Many walls carbon nanometer tube of 0.09 gram is dispersed in 50 milliliters the ethylene glycol solution that contains 0.00005 mole of palladium bichloride uniformly, and heating is 1 minute under 700 watts microwave radiation.The average grain diameter of the nanometer cake particle of transmission electron microscope observing carbon nanometer tube area load is at 3.8nm, and grain is through being distributed between the 2-4.2nm, and metal nanoparticle is 5.5% in the load capacity of carbon nano tube surface.And with the average grain diameter of the nanometer platinum particles of the carbon nanometer tube load of traditional immersion-method of reducing preparation at 6.8nm, grain is through being distributed between the 1-12.3nm.
Embodiment 7:
Many walls carbon nanometer tube of 0.09 gram is dispersed in 50 milliliters the ethylene glycol solution that contains 0.00005 mole of gold chloride uniformly, and heating is 1 minute under 700 watts microwave radiation.The average grain diameter of the nano Au particle of transmission electron microscope observing carbon nanometer tube area load is at 3.5nm, and grain is through being distributed between the 2-4nm, and metal nanoparticle is 10% in the load capacity of carbon nano tube surface.And with the average grain diameter of the nanometer platinum particles of the carbon nanometer tube load of traditional immersion-method of reducing preparation at 7.6nm, grain is through being distributed between the 2-11nm.
Embodiment 8:
Many walls carbon nanometer tube of 0.04 gram is dispersed in 50 milliliters the ethylene glycol solution that contains 0.00005 equimolar silver nitrate uniformly, and heating is 1 minute under 700 watts microwave radiation.The average grain diameter of the nanometer ruthenium particle of transmission electron microscope observing carbon nanometer tube area load is at 3.4nm, and grain is through being distributed between the 2-4nm, and the ruthenium metal nanoparticle is 11% in the load capacity of carbon nano tube surface.And with the average grain diameter of the nanometer platinum particles of the carbon nanometer tube load of traditional immersion-method of reducing preparation at 6.0nm, grain is through being distributed between the 1-9nm.
Claims (4)
1. the method at carbon nanometer tube area load nano metal particles is characterized in that even carbon nanotube is dispersed in the slaine polyhydric alcohol solutions, adopts the homogeneous mixture of this CNT of carry out microwave radiation heating and slaine polyhydric alcohol solutions then; The polyhydric alcohol solutions of per 1 liter slaine contains 0.2～8 gram CNT; The concentration of slaine is 0.0002～0.03 mol in the slaine polyhydric alcohol solutions.
2. according to the described a kind of method of claim 1, it is characterized in that said slaine is: chloroplatinic acid, potassium chloroplatinate, platinum acetate, ruthenic chloride, gold chloride, silver nitrate, palladium bichloride, palladium at carbon nanometer tube area load nano metal particles; The metal of institute's load is on CNT accordingly: Pt, Pd, Ru, Au, Ag.
3. according to the described a kind of method of claim 1, it is characterized in that said polyalcohol is an ethylene glycol at carbon nanometer tube area load nano metal particles.
4, according to the described a kind of method of claim 1, it is characterized in that said CNT is: multi-walled carbon nano-tubes or SWCN at carbon nanometer tube area load nano metal particles.
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