CN103882388A - Preparation method of nano-composite Ag/CNTs one-dimensional material - Google Patents
Preparation method of nano-composite Ag/CNTs one-dimensional material Download PDFInfo
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- CN103882388A CN103882388A CN201410064633.9A CN201410064633A CN103882388A CN 103882388 A CN103882388 A CN 103882388A CN 201410064633 A CN201410064633 A CN 201410064633A CN 103882388 A CN103882388 A CN 103882388A
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Abstract
The invention provides a preparation method of a nano-composite Ag/CNTs one-dimensional material. The preparation method disclosed by the invention comprises the following steps of: firstly, immersing a carbon nano tube in ethanol or acetone, after carrying out ultrasonic dispersion treatment, spraying the carbon nano tube on a matrix, and drying at 60 DEG C; and then, putting the matrix sprayed with the carbon nano tube on a sample table in an ion sputtering apparatus, taking Ag as the target sputtering electrode, sputtering for 10 s to 2 min with the sputtering vacuum degree of (10-1)-(10-3) Mpa and the sputtering current of 10-30 mA, and obtaining the nano-composite Ag/CNTs one-dimensional material with the nano-silver-to-CNTs mass ratio of 0.1 to 4.1. The preparation method of the nano-composite Ag/CNTs one-dimensional material disclosed by the invention is simple and controllable in preparation process, rapid in finished product rate and low in cost; and the nano-composite Ag/CNTs one-dimensional material having good dispersity and high loading capacity can be obtained.
Description
Technical field
The invention belongs to Material Field, the preparation method of especially nano combined Ag/CNTs one-dimensional material.
Background technology
Silver nano-grain is with a wide range of applications in fields such as fuel cell, photosensor, biomaterials.But in these application, be often faced with a common problem, i.e. the reduction of Nano silver grain easy chemistry of reuniting and cause thus, optics, catalytic performance in the time of high-content.In order to realize high-content, low reunion this purpose, part Study personnel utilize the good erosion resistance of carbon support, the advantages such as biocompatibility and high specific surface area, synthesize carbon back supported silver nano-particle material, as Ag/ saccharan [P.Sanpui.ACS Appl, Mater.Interfaces, 3 (2011) 218-228], Ag/ Graphene [S.Bong.Electrochem.Commun.12 (2010) 129-131], Ag/ carbon black [Xinhua Xu.J.Electroanalytical Chemistry, 696 (2013) 9-14], Ag/CNTs(An Ting etc., Acta PhySico-Chimica Sinica, 2012, 28 (9), 2202-2208) etc., improve to a certain extent the dispersed and active of silver particles, but due to its preparation method, as chemical deposition and electroless plating method, hydrothermal method, the limitation of the liquid phase methods such as silver mirror method, make the charge capacity of Ag nano particle conventionally very low, if raising charge capacity, there is agglomeration in Ag nano particle, be difficult to meet in practical application to Ag nano particle high dispersive, the requirement of high capacity amount.[the Journal of Inorganic Materials such as Wu Yongqing, 2009,24:122-144] adopt simple thermal evaporation sedimentation to synthesize Ag nano-crystalline granule/multi-wall carbon nano-tube composite material, but this method Ag target temperature is up to 1000 ℃, nanometer silver is oxidizable, and easily causes carbon nanotube generation deformation.
Summary of the invention
In order to overcome above-mentioned preparation method's shortcoming, the invention provides the preparation method of a kind of simple process, Ag nanoparticulate dispersed is good, charge capacity is large nano combined Ag/CNTs one-dimensional material.
The object of the invention is to be achieved through the following technical solutions:
A preparation method for nano combined Ag/CNTs one-dimensional material, is characterized in that, comprises the following steps:
(1) carbon nanotube (be called for short " CNTs ") is immersed in ethanol or acetone, utilize after ultrasonic dispersion treatment, be sprayed on matrix, dry at 60 ℃;
(2) matrix that has sprayed carbon nanotube is placed in the sample table of ion sputtering instrument, take Ag as target sputtering electrode, in sputter vacuum tightness 10
-1~10
-3under the condition that Mpa, sputtering current are 10~30mA, sputter 10s~2min, the nano combined Ag/CNTs one-dimensional material that the mass ratio that obtains nanometer silver and CNTs is 0.1~4:1.
Preferably, matrix described in step (1) is sheet glass or PET(full name " polyethylene terephthalate ") film.
Preferably, sputter vacuum tightness 10 in step (2)
-2under the condition that Mpa, sputtering current are 10mA, sputtering time is 2min.
Preferably, sputter vacuum tightness 10 in step (2)
-1under the condition that Mpa, sputtering current are 20mA, sputtering time is 1.2min.
Preferably, sputter vacuum tightness 10 in step (2)
-3under the condition that Mpa, sputtering current are 30mA, sputtering time is 10s.
Preparation method's tool of the present invention has the following advantages:
(1) preparation process is simply controlled, and finished product speed is fast, and cost is low.
(2) because the specific surface area of carbon nanotube is large, nano-silver loaded is on its surface, and charge capacity is large, dispersed high, active strong.
Accompanying drawing explanation
Fig. 1 characterizes the SEM photo that is sprayed on the CNTs surface topography on matrix.
Fig. 2 is the SEM photo that characterizes the nano combined Ag/CNTs one-dimensional material surface topography that obtains of embodiment 1.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to this.
Embodiment 1:
First, CNTs is immersed in ethanol, supersound process, after 10 minutes, is sprayed on sheet glass, dry at 60 ℃.Then, the sheet glass that is coated with CNTs is positioned in the sample table in Japanese JFC-1600 ion sputtering instrument, take Ag target as sputtering electrode, is evacuated to vacuum tightness 10
-2mpa stops, and sputter 2min under sputtering current 10mA obtains nano combined Ag/CNTs one-dimensional material.
Adopt the Japanese JEOL JSM-7001F of company field emission scanning electron microscope, obtain the surface topography that characterizes the nano combined Ag/CNTs one-dimensional material for preparing of embodiment 1, as shown in Figure 2.Compared with the surface topography of the CNTs shown in Fig. 1, the preparation method described in embodiment 1 in the surface uniform load of CNTs silver nano-grain.Nano combined Ag/CNTs one-dimensional material surface in SEM viewing area, gets arbitrarily 3 points and carries out energy spectrum analysis, the results are shown in Table 1, and EDAX results shows that the mass ratio of Ag:C is about 4:1.
Embodiment 2:
First, CNTs is immersed in acetone, supersound process, after 30 minutes, is sprayed on PET film, dry at 60 ℃, then, the PET film that is coated with CNTs is positioned in the sample table in ion sputtering instrument, and sputtering electrode is Ag target, is evacuated to vacuum tightness 10
-1mpa stops, and sputtering time 1.2min under sputtering current 20mA obtains nano combined Ag/CNTs one-dimensional material.Test result shows: the preparation method described in embodiment 2 in the surface uniform load of CNTs silver nano-grain; EDAX results: Ag:C mass ratio is about 2:1.
Embodiment 3:
First, CNTs is immersed in ethanol, supersound process, after 20 minutes, is sprayed on PET film, dry at 60 ℃.Then, the PET film that is coated with CNTs is positioned in the sample table in ion sputtering instrument, sputtering electrode is Ag target, is evacuated to vacuum tightness 10
-3mpa stops, and sputtering time 10s under sputtering current 30mA obtains nano combined Ag/CNTs one-dimensional material.Result shows: the preparation method described in embodiment 3 in the surface uniform load of CNTs silver nano-grain; EDAX results: Ag:C mass ratio is about 0.1:1.
The Ag/C mass ratio on the table 1 embodiment nano combined Ag/CNTs one-dimensional material of 1~3 gained surface
Above-described embodiment is preferred embodiment of the present invention; but the present invention is not limited to above-mentioned embodiment; in the situation that not deviating from flesh and blood of the present invention, any apparent improvement, replacement or modification that those skilled in the art can make all belong to protection scope of the present invention.
Claims (5)
1. a preparation method for nano combined Ag/CNTs one-dimensional material, is characterized in that, comprises the following steps:
(1) carbon nanotube is immersed in ethanol or acetone, utilize after ultrasonic dispersion treatment, be sprayed on matrix, dry at 60 ℃;
(2) matrix that has sprayed carbon nanotube is placed in the sample table of ion sputtering instrument, take Ag as target sputtering electrode, in sputter vacuum tightness 10
-1~10
-3under the condition that Mpa, sputtering current are 10~30mA, sputter 10s~2min, the nano combined Ag/CNTs one-dimensional material that the mass ratio that obtains nanometer silver and CNTs is 0.1~4:1.
2. the preparation method of nano combined Ag/CNTs one-dimensional material according to claim 1, is characterized in that, matrix described in step (1) is sheet glass or PET film.
3. the preparation method of nano combined Ag/CNTs one-dimensional material according to claim 1, is characterized in that, sputter vacuum tightness 10 in step (2)
-2under the condition that Mpa, sputtering current are 10mA, sputtering time is 2min.
4. the preparation method of nano combined Ag/CNTs one-dimensional material according to claim 1, is characterized in that, sputter vacuum tightness 10 in step (2)
-1under the condition that Mpa, sputtering current are 20mA, sputtering time is 1.2min.
5. the preparation method of nano combined Ag/CNTs one-dimensional material according to claim 1, is characterized in that, sputter vacuum tightness 10 in step (2)
-3under the condition that Mpa, sputtering current are 30mA, sputtering time is 10s.
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Citations (1)
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---|---|---|---|---|
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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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 |
Non-Patent Citations (3)
Title |
---|
吴永庆,等: "Ag纳米晶颗粒/碳纳米管复合材料的制备与结构研究", 《无机材料学报》 * |
张洁,等: "碳纳米管和金属纳米粒子复合结构的拉曼光谱特性", 《中国激光》 * |
闫晓琦,等: "溅射镀Au-CNTs复合材料的制备及电化学储氢性能", 《中国有色金属学报》 * |
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Application publication date: 20140625 |