CN1150997C - Method for coating mono-metal particles on carbon nano tube surface - Google Patents
Method for coating mono-metal particles on carbon nano tube surfaceInfo
- Publication number
- CN1150997C CN1150997C CNB021601917A CN02160191A CN1150997C CN 1150997 C CN1150997 C CN 1150997C CN B021601917 A CNB021601917 A CN B021601917A CN 02160191 A CN02160191 A CN 02160191A CN 1150997 C CN1150997 C CN 1150997C
- Authority
- CN
- China
- Prior art keywords
- carbon nano
- tubes
- slaine
- tube surface
- nano tube
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 46
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000002923 metal particle Substances 0.000 title description 4
- 239000011248 coating agent Substances 0.000 title 1
- 238000000576 coating method Methods 0.000 title 1
- 239000002245 particle Substances 0.000 claims abstract description 27
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 17
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 15
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 14
- 230000005855 radiation Effects 0.000 claims abstract description 10
- 229910052709 silver Inorganic materials 0.000 claims abstract description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims abstract description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 36
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 24
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000002048 multi walled nanotube Substances 0.000 claims description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 4
- CTUFHBVSYAEMLM-UHFFFAOYSA-N acetic acid;platinum Chemical compound [Pt].CC(O)=O.CC(O)=O CTUFHBVSYAEMLM-UHFFFAOYSA-N 0.000 claims description 3
- 239000008240 homogeneous mixture Substances 0.000 claims description 2
- 239000013528 metallic particle Substances 0.000 abstract description 6
- 150000003839 salts Chemical class 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- 239000002082 metal nanoparticle Substances 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 5
- 239000010944 silver (metal) Substances 0.000 description 4
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 229910052707 ruthenium Inorganic materials 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- ZODDGFAZWTZOSI-UHFFFAOYSA-N nitric acid;sulfuric acid Chemical compound O[N+]([O-])=O.OS(O)(=O)=O ZODDGFAZWTZOSI-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- QCSGLAMXZCLSJW-UHFFFAOYSA-L platinum(2+);diacetate Chemical compound [Pt+2].CC([O-])=O.CC([O-])=O QCSGLAMXZCLSJW-UHFFFAOYSA-L 0.000 description 1
- 238000004917 polyol method Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Catalysts (AREA)
Abstract
The present invention discloses a method for carrying nanometer monometallic particles on the surfaces of carbon nano-tubes, and metal is Pt, Pd, Ru, Au and Ag. The carbon nano-tubes are uniformly dispersed in a polyalcohol solution of one kind of metallic salts, and uniform mixtures of the carbon nano-tubes and the polyalcohol solution of the metallic salts are heated by microwave radiation; 1 liter of polyalcohol solution of the metallic salts contains 0.2 to 8g of carbon nano-tube; the concentration of the metallic salts of the polyalcohol solution of the metallic salts is from 0.0002 to 0.03 mol/l; the carried quantity of the metallic particles on the surfaces of the carbon nano-tubes is from 5% to 42%. The present invention has the advantages that the nanometer metallic particles carried on the surfaces of the carbon nano-tubes have small particle size, the average particle size of the nanometer metallic particles is from 3 to 4 nm, and the nanometer metallic particles have narrow particle size distribution. The present invention also has the advantages of rapidity, simplicity and high efficiency, and the materials of the nanometer metallic particles carried on the carbon nano-tubes have extensive application in the fields of electrochemical energy transfer and catalysis.
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 particle.
Background technology
CNT 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 at metallics such as carbon nano tube surface supporting Pt and Ru.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 CNT after handling is immersed in the solution that contains slaine, make slaine be adsorbed on the surface (the interior pipe that enters CNT is also arranged) of CNT, 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 the reducing agent of ethylene glycol generation at high temperature makes the metal ion reduction 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 nano tube surface loaded with nano 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; Slaine is: chloroplatinic acid, potassium chloroplatinate, platinum acetate, ruthenic chloride, gold chloride, silver nitrate, palladium bichloride=or palladium; The metal of institute's load is on CNT accordingly: Pt, Pd, Ru, Au=or Ag; Polyalcohol is an ethylene glycol.
Advantage of the present invention is tiny at the Pt of carbon nano tube surface load, Pd, Ru, Au or Ag metal nanoparticle particle diameter, 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 material of this carbon nanotube loaded metal nanoparticle 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 or palladium; Polyalcohol is an ethylene glycol; CNT is multi-walled carbon nano-tubes or SWCN.
Embodiment 1:
The multi-walled carbon nano-tubes of 0.08 gram is dispersed in 50 milliliters the ethylene glycol solution that contains 0.0001 mole of chloroplatinic acid 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 nano tube surface load is at 3.5nm, and grain is through being distributed between the 2-4nm. and platinum nanoparticles is 19% in the load capacity of carbon nano tube surface.And with the average grain diameter of the carbon nanotube loaded nanometer platinum particles of traditional immersion-method of reducing preparation at 7.6nm, grain is through being distributed between the 2-11nm.
Embodiment 2:
The SWCN 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 nano tube surface 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 carbon nanotube loaded nanometer platinum particles of traditional immersion-method of reducing preparation at 6.6nm, grain is through being distributed between the 1-9nm.
Embodiment 3:
The multi-walled carbon nano-tubes 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 nano tube surface 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 carbon nanotube loaded nanometer platinum particles of traditional immersion-method of reducing preparation at 7.8nm, grain is through being distributed between the 1-13nm.
Embodiment 4:
The multi-walled carbon nano-tubes of 0.02 gram is dispersed in 50 milliliters the ethylene glycol solution that contains 0.00005 mole of ruthenic chloride uniformly, heating is 1 minute under 700 watts microwave radiation. and the average grain diameter of the nanometer ruthenium particle of transmission electron microscope observing carbon nano tube surface load is at 3.2nm, 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 carbon nanotube loaded nanometer ruthenium particle of traditional immersion-method of reducing preparation at 6.1nm, grain is through being distributed between the 1-9nm.
Embodiment 5:
The multi-walled carbon nano-tubes of 0.09 gram is dispersed in 50 milliliters the ethylene glycol solution that contains 0.00005 molar acetate palladium uniformly, heating is 1 minute under 700 watts microwave radiation. and the average grain diameter of the nanometer palladium particle of transmission electron microscope observing carbon nano tube surface load is at 3.8nm, grain is through being distributed between the 2-4.2nm, and the palladium metal nano particle is 5.5% in the load capacity of carbon nano tube surface.And with the average grain diameter of the carbon nanotube loaded nanometer palladium particle of traditional immersion-method of reducing preparation at 6.8nm, grain is through being distributed between the 1-12.3nm.
Embodiment 6:
The multi-walled carbon nano-tubes of 0.09 gram is dispersed in 50 milliliters the ethylene glycol solution that contains 0.00005 mole of gold chloride uniformly, heating is 1 minute under 700 watts microwave radiation. and the average grain diameter of the nano Au particle of transmission electron microscope observing carbon nano tube surface load is at 3.5nm, 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 carbon nanotube loaded nano Au particle of traditional immersion-method of reducing preparation at 7.6nm, grain is through being distributed between the 2-11nm.
Embodiment 7:
The multi-walled carbon nano-tubes 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 nano silver particles of transmission electron microscope observing carbon nano tube surface load is at 3.4nm, and grain is through being distributed between the 2-4nm, and the silver metal nano particle is 11% in the load capacity of carbon nano tube surface.And with the average grain diameter of the carbon nanotube loaded nano silver particles of traditional immersion-method of reducing preparation at 6.0nm, grain is through being distributed between the 1-9nm.
Claims (2)
1. the method at carbon nano tube surface loaded with nano monometallic particle 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, and slaine is: chloroplatinic acid, potassium chloroplatinate, platinum acetate, ruthenic chloride, gold chloride, silver nitrate, palladium bichloride or palladium; The metal of institute's load is on CNT accordingly: Pt, Pd, Ru, Au or Ag, polyalcohol are ethylene glycol.
2, 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 nano tube surface loaded with nano monometallic particle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021601917A CN1150997C (en) | 2002-12-27 | 2002-12-27 | Method for coating mono-metal particles on carbon nano tube surface |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021601917A CN1150997C (en) | 2002-12-27 | 2002-12-27 | Method for coating mono-metal particles on carbon nano tube surface |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1424149A CN1424149A (en) | 2003-06-18 |
| CN1150997C true CN1150997C (en) | 2004-05-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB021601917A Expired - Fee Related CN1150997C (en) | 2002-12-27 | 2002-12-27 | Method for coating mono-metal particles on carbon nano tube surface |
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2002
- 2002-12-27 CN CNB021601917A patent/CN1150997C/en not_active Expired - Fee Related
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