CN101445911B - Method for preparing monodispersed Cu nanoparticle template by using secondary evaporation method - Google Patents
Method for preparing monodispersed Cu nanoparticle template by using secondary evaporation method Download PDFInfo
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- CN101445911B CN101445911B CN2008102292992A CN200810229299A CN101445911B CN 101445911 B CN101445911 B CN 101445911B CN 2008102292992 A CN2008102292992 A CN 2008102292992A CN 200810229299 A CN200810229299 A CN 200810229299A CN 101445911 B CN101445911 B CN 101445911B
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Abstract
The invention provides a method for preparing a monodispersed Cu nanoparticle template by using the secondary evaporation method, and the method is mainly technically characterized in that the temperature is constant at 1300 DEG C for 40-60min in 300Torr nitrogen atmosphere to evaporate Cu powder, so that a layer of Cu is evenly covered on a smooth and clean adamant sleeve; the adamant sleeve obtained by evaporation is taken as a Cu source for secondary evaporation, a P-111 type Si wafer is taken as a substrate, flowing Ar gas is used for protection, the flow rate of the gas is 100sccm, and the temperature is constant at 1300 DEG C for 30-50min, so as to prepare the monodispersed Cu nanoparticle template. The method has the advantages that the deposition process is even and stable, the monodispersion of nanoparticles is good, the method solves the difficult problem that the conventional physical and chemical dispersion methods can not completely disperse the nanoparticles, and the method can further effectively control the particle size, the dispersion density and the coverage rate by regulating the experimental temperature, the constant temperature time and the flow rate of the gas.
Description
Technical field:
The present invention relates to the monodispersed method of a kind of metal nanoparticle, particularly a kind of method that is equipped with monodispersed Cu nanoparticle template with the double evaporation-cooling legal system.
Background technology:
Current, along with the continuous development of various monodimension nanometer material technologies of preparing, metal nanoparticle has produced brand-new purposes, can be used as the catalyzer seed pattern exactly, promotes the oriented growth of one dimension Nano structure.The fusing point of Cu is 1083 ℃, and is suitable with the preparation temperature of one dimension semiconductor nano wire, so it is difficult for evaporation during as catalyzer.So just require nano particle to possess very high single degree of scatter; In addition, the size that also requires nano particle is below 100nm, and size distribution is even; Particulate divides bulk density will try one's best greatly, thereby guarantees the fraction of coverage of whole template.
The nanoparticulate dispersed method mainly is divided into the physics dispersion at present, as mechanical stirring, ultrasonic vibration etc. and chemical dispersion, adds dispersion agent, changes particle surface character.But all only be the reunion that the reunion of a large amount of nanoparticles is transformed into a small amount of nanoparticle, or the single of part nanoparticle disperses, dispersive ability is not strong, does not reach complete monodispersed degree.
Summary of the invention:
The objective of the invention is the deficiency that exists in the above-mentioned technology, a kind of method that is equipped with monodispersed Cu nanoparticle template with the double evaporation-cooling legal system is provided.
By double evaporation-cooling, improved the homogeneity of heating evaporation, make deposition process uniform and stable, can access monodispersed individual layer Cu nanoparticle template.
The object of the present invention is achieved like this: it is characterized in that: the corundum porcelain boat that (1) will fill the Cu powder of the purity 99.9% corundum sleeve pipe of packing into, and at 1300 ℃, 300Torr N
2Be incubated 40-60min under the condition of gas, the telescopic inwall last layer Cu that distributes uniformly; (2) the corundum sleeve pipe that obtains of evaporation is substrate as the Cu source of evaporation for the second time with P-111 type Si sheet, the Ar gas shiled of flowing, and gas flow rate 100sccm at 1300 ℃ of constant temperature 30-50min of temperature, prepares monodispersed Cu nanoparticle template.
Advantage of the present invention is, deposition process is uniform and stable, the monodispersity of nano particle is good, the template of preparation satisfies the requirement of oriented growth one dimension semiconductor nano material, solved a thoroughly dispersing nanometer particulate difficult problem of conventional physics, chemical dispersion method, and can effectively control particle size, divide bulk density and fraction of coverage by regulating experimental temperature, constant temperature time and gas flow rate, so this method be a kind of very effective preparation monodispersed Cu nanoparticle template method.
Description of drawings:
Fig. 1 is the electron scanning micrograph with the template of this method preparation
Fig. 2 is the particle size distribution figure of Cu nano particle on the template
Fig. 3 is the energy spectrogram of this template
Embodiment:
Embodiment is: the corundum porcelain boat that the first step will fill the Cu powder of the purity 99.9% corundum sleeve pipe of packing into, sleeve pipe together with the porcelain boat thermal center (-tre) that adds of electric tube furnace of being rapidly heated of packing into, at 1300 ℃, 300TorrN
2Be incubated 40-60min under the condition of gas, the telescopic inwall last layer Cu that then can distribute uniformly is as the Cu source of step evaporation down; Second step is being of a size of 1cm
2P-111 type Si sheet through the cleaned by ultrasonic vibration of 10min; place the inner sleeve after the step handles; then under mobile Ar gas shiled; gas flow rate 100sccm; speed with 25 ℃/min causes 1300 ℃ with the boiler tube intensification, constant temperature 30-50min, and the boiler tube naturally cooling causes room temperature; take out the Si sheet after passivation 4-8 hour, promptly obtain monodispersed Cu nanoparticle template.
Template finished put into the JSM-6301F field emission scanning electron microscope after the metal spraying process and carry out microscopic appearance and observe, and utilize the Oxford energy spectrometer to carry out the Chemical Composition analysis.Fig. 1 as can be seen on the template particle be and arrange single the dispersion, particle size is even, size distribution 23-96nm, average 54nm divides bulk density 1.96 * 10
10/ cm
2, fraction of coverage 45%.Fig. 2 particle diameter has as can be seen occupied 83% at the amounts of particles of 40-70nm, and very the grain diameter of minority is below the 40nm or more than the 70nm, the particle size uniformity excellence of this sample.Fig. 3 nanoparticle on the template as can be seen is Cu, and the metal spraying process of the peak of Si, O, three kinds of elements of Au when deriving from CuO film that Si substrate, Cu nano particle passivation rear surface form and preparation SEM sample respectively.
Claims (2)
1. one kind is equipped with the method for monodispersed Cu nanoparticle template with the double evaporation-cooling legal system, it is characterized in that,
(1) the corundum porcelain boat that will fill the Cu powder of the purity 99.9% corundum sleeve pipe of packing into is at 1300 ℃, 300TorrN
2Be incubated 40-60min under the condition of gas, the telescopic inwall last layer Cu that distributes uniformly;
(2) the corundum sleeve pipe that obtains of evaporation is substrate as the Cu source of evaporation for the second time with P-111 type Si sheet, the Ar gas shiled of flowing, and gas flow rate 100sccm at 1300 ℃ of constant temperature 30-50min of temperature, prepares monodispersed Cu nanoparticle template.
2. according to claim 1ly a kind ofly be equipped with the method for monodispersed Cu nanoparticle template, it is characterized in that the template surface Cu nano particle of preparing is arranges single the dispersion with the double evaporation-cooling legal system, particle size is even, size distribution 23-96nm, average 54nm divides bulk density 1.96 * 10
10/ cm
2, fraction of coverage 45%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2008102292992A CN101445911B (en) | 2008-12-05 | 2008-12-05 | Method for preparing monodispersed Cu nanoparticle template by using secondary evaporation method |
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| CN2008102292992A CN101445911B (en) | 2008-12-05 | 2008-12-05 | Method for preparing monodispersed Cu nanoparticle template by using secondary evaporation method |
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| CN101445911A CN101445911A (en) | 2009-06-03 |
| CN101445911B true CN101445911B (en) | 2010-07-14 |
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| CN2008102292992A Expired - Fee Related CN101445911B (en) | 2008-12-05 | 2008-12-05 | Method for preparing monodispersed Cu nanoparticle template by using secondary evaporation method |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101255544A (en) * | 2008-03-21 | 2008-09-03 | 中国科学院上海硅酸盐研究所 | Method for preparing nano metal or metal oxide/carbon nano-tube composite material |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101255544A (en) * | 2008-03-21 | 2008-09-03 | 中国科学院上海硅酸盐研究所 | Method for preparing nano metal or metal oxide/carbon nano-tube composite material |
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