CN109573984A - The preparation method of nano silver composite carbon nanometer tube - Google Patents
The preparation method of nano silver composite carbon nanometer tube Download PDFInfo
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- CN109573984A CN109573984A CN201811636669.4A CN201811636669A CN109573984A CN 109573984 A CN109573984 A CN 109573984A CN 201811636669 A CN201811636669 A CN 201811636669A CN 109573984 A CN109573984 A CN 109573984A
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- silver
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- carbon nanotube
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
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- 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
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/24—Thermal properties
Abstract
A kind of preparation method of advanced material technical field nano silver composite carbon nanometer tube, comprising the following steps: carbon nanotube and silver salt solution are mixed and made into composite mortar first, later dry compacting；Again by after compacting carbon nanotube and silver salt connect with a pair of of graphite electrode after vacuumize；Then pulse current is passed through under vacuum condition, carbon nanotube and silver salt to the silver salt after heating compacting are pyrolyzed, and form nano-Ag particles in carbon nano tube surface；Finally lead to inert gas purge impurity and cool down and completes the preparation of nano silver composite carbon nanometer tube.The present invention utilizes the good capacity of heat transmission of carbon nanotube and chemical stability, the high-efficiency heating to carbon nanotube and silver salt mixture is realized by pulse current, without heat-conducting medium and ambient heat, the silver salt fast pyrogenation for adhering to carbon nano tube surface forms subtle silver-colored crystal grain, realizes the quick preparation of nano silver composite carbon nanometer tube.
Description
Technical field
The present invention relates to a kind of technology in advanced material field, the system of specifically a kind of nano silver composite carbon nanometer tube
Preparation Method.
Background technique
What nano silver composite carbon nanometer tube material combined nano silver and carbon nanotube cooperates with advantage, has small size effect
It answers, quantum size effect, skin effect and macro quanta tunnel effect, integrates the performances such as antibacterial, catalysis, conduction, thermally conductive,
It has broad application prospects.Chemical plating is to prepare the common method of nano silver composite carbon nanometer tube material, but this method needs
Carbon nanotube is pre-processed using oxidation, sensitization, activating process, improve the activation capacity of carbon nanotube, it is also necessary to adjust
Whole plating solution composition, temperature, pH value, process complicated and time consumption, contaminated wastewater processing cost is high, and control of product quality is difficult.
Summary of the invention
The present invention In view of the above shortcomings of the prior art, proposes a kind of preparation side of nano silver composite carbon nanometer tube
Method is realized mixed to carbon nanotube and silver salt using the good capacity of heat transmission of carbon nanotube and chemical stability by pulse current
The high-efficiency heating for closing object, without heat-conducting medium and ambient heat, the silver salt fast pyrogenation for adhering to carbon nano tube surface is formed
Subtle silver crystal grain, realizes the quick preparation of nano silver composite carbon nanometer tube.
The present invention is achieved by the following technical solutions:
The present invention the following steps are included:
Carbon nanotube and silver salt solution are mixed and made into composite mortar first, later dry compacting；
The carbon nanotube after compacting is connect with silver salt with a pair of of graphite electrode again, is vacuumized later, the carbon after making compacting
Nanotube and silver salt are under vacuum condition；
Then pulse current is passed through under vacuum condition, carbon nanotube and silver salt to the silver salt after heating compacting are pyrolyzed,
Carbon nano tube surface forms nano-Ag particles；
Finally lead to inert gas purge impurity and cool down and completes the preparation of nano silver composite carbon nanometer tube.
The silver salt is silver acetate, silver nitrate, any one in silver sulfate.
The molar ratio of the silver salt and carbon nanotube is 0.1-2.0:1.0.
The pulse current is 10mA-100A, burst length 0.1-10s.
The heating temperature is 200-500 DEG C.
The partial size of the nano-Ag particles is 5-100nm.
Technical effect
Compared with prior art, the present invention utilizes the good capacity of heat transmission of carbon nanotube and chemical stability, passes through pulse
Electric current makes carbon nanotube generate amount of heat (Q=I2Rt), to silver salt high-efficiency heating, without heat-conducting medium and ambient heat,
The silver salt fast pyrogenation for adhering to carbon nano tube surface forms subtle silver-colored crystal grain, realizes the quick system of nano silver composite carbon nanometer tube
It is standby.
Detailed description of the invention
Fig. 1 is the SEM photograph of crystal whisker-shaped multi-walled carbon nanotube in embodiment 1；
Fig. 2 is the SEM photograph of nano silver composite carbon nanometer tube in embodiment 1.
Specific embodiment
With reference to the accompanying drawing and specific embodiment the present invention will be described in detail.
The embodiment of the present invention includes following steps:
Carbon nanotube and silver salt solution are mixed and made into composite mortar first, later dry compacting；
The carbon nanotube after compacting is connect with silver salt with a pair of of graphite electrode again, is vacuumized later, the carbon after making compacting
Nanotube and silver salt are under vacuum condition；
Then pulse current is passed through under vacuum condition, carbon nanotube and silver salt to the silver salt after heating compacting are pyrolyzed,
Carbon nano tube surface forms nano-Ag particles；
Finally lead to argon gas purging impurity and cool down and completes the preparation of nano silver composite carbon nanometer tube.
The silver salt is silver acetate, silver nitrate, any one in silver sulfate；Preferably, using silver acetate.
The molar ratio of the silver acetate and carbon nanotube is 0.1-2.0:1.0.
The pulse current is 10mA-100A, burst length 0.1-10s.
The heating temperature is 200-500 DEG C.
The partial size of the nano-Ag particles is 5-100nm.
Embodiment 1
The present embodiment the following steps are included:
S1, 2kg silver acetate is dissolved in 20L water, 144g crystal whisker-shaped multi wall carbon is then added into silver acetate aqueous solution
(Suzhou the first element Nanosolutions GmbH, 5-10 μm long, diameter 50-90nm, purity is greater than 99% to nanotube, such as Fig. 1 institute
Show)；It under ultrasonication, is uniformly mixed carbon nanotube with silver acetate aqueous solution, forms silver acetate-carbon nanotube composite pulp
Material；Silver acetate-carbon nanotube composite dry powder is made by 80 DEG C of vacuum drying in silver acetate-carbon nanotube composite mortar again；
S2, silver acetate-carbon nanotube composite dry powder is compacted, then is connect with a pair of of graphite electrode；Then it vacuumizes, logical argon
Gas repetitive operation 3 times, thoroughly excludes air, then vacuumize, and is in silver acetate-carbon nanotube composite dry powder under vacuum condition,
Vacuum degree is maintained at 9.0 × 10-8mbar；
S3, using pulse electric heating mode, the size of current for being passed through pulse current is 1A, and current impulse is in 1s to acetic acid
Silver-carbon nanotube composite dry powder generates joule thermal shock, and the temperature of carbon nanotube is sharply increased to 300 DEG C, and silver acetate is in high temperature
Under ultrafast thermal decomposition, carbon nano tube surface generate silver nano-grain；
S4, finally lead to argon gas purging impurity and cool down, to obtain the nano silver composite carbon nanometer tube of high-purity.
Nano silver composite carbon nanometer tube is made to the present embodiment by scanning electron microscope and carries out structural characterization, obtains figure
The figure of SEM shown in 2.From the SEM of Fig. 2 figure as can be seen that carbon nanotube dispersion effect is preferable, soilless sticking phenomenon；The crystal grain of nano silver
Size is evenly distributed in carbon nano tube surface in 40nm or so.
It is emphasized that: the above is only presently preferred embodiments of the present invention, not make in any form to the present invention
Limitation, any simple modification, equivalent change and modification to the above embodiments according to the technical essence of the invention,
All of which are still within the scope of the technical scheme of the invention.
Claims (6)
1. a kind of preparation method of nano silver composite carbon nanometer tube, which comprises the following steps:
Carbon nanotube and silver salt solution are mixed and made into composite mortar first, later dry compacting；
Again by after compacting carbon nanotube and silver salt connect with a pair of of graphite electrode, vacuumize later, make the carbon nanometer after being compacted
Pipe is under vacuum condition with silver salt；
Then pulse current is passed through under vacuum condition, carbon nanotube and silver salt to the silver salt after heating compacting are pyrolyzed, and are received in carbon
Nanotube surface forms nano-Ag particles；
Finally lead to inert gas purge impurity and cool down and completes the preparation of nano silver composite carbon nanometer tube.
2. the preparation method of nano silver composite carbon nanometer tube according to claim 1, characterized in that the silver salt is acetic acid
Silver, silver nitrate, any one in silver sulfate.
3. the preparation method of nano silver composite carbon nanometer tube according to claim 2, characterized in that the silver salt and carbon nanometer
The molar ratio of pipe is 0.1-2.0:1.0.
4. the preparation method of nano silver composite carbon nanometer tube according to claim 1, characterized in that the pulse current is
10mA-100A, burst length 0.1-10s.
5. the preparation method of nano silver composite carbon nanometer tube according to claim 1, characterized in that the heating temperature is
200-500℃。
6. the preparation method of nano silver composite carbon nanometer tube according to claim 1, characterized in that the nano-Ag particles
Partial size is 5-100nm.
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| CN201811636669.4A CN109573984A (en) | 2018-12-29 | 2018-12-29 | The preparation method of nano silver composite carbon nanometer tube |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112170861A (en) * | 2020-09-30 | 2021-01-05 | 桂林金格电工电子材料科技有限公司 | Preparation method of silver tungsten carbide contact material |
| CN114455586A (en) * | 2022-02-22 | 2022-05-10 | 合肥工业大学 | W-shaped steel plate2Rapid preparation method of C nanoparticles |
| CN114497567A (en) * | 2022-03-07 | 2022-05-13 | 中船重工黄冈水中装备动力有限公司 | Silver/carbon nanotube composite material for aluminum-silver oxide battery and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112170861A (en) * | 2020-09-30 | 2021-01-05 | 桂林金格电工电子材料科技有限公司 | Preparation method of silver tungsten carbide contact material |
| CN114455586A (en) * | 2022-02-22 | 2022-05-10 | 合肥工业大学 | W-shaped steel plate2Rapid preparation method of C nanoparticles |
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| CN114497567A (en) * | 2022-03-07 | 2022-05-13 | 中船重工黄冈水中装备动力有限公司 | Silver/carbon nanotube composite material for aluminum-silver oxide battery and preparation method and application thereof |
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Address after: Room 105 and 207, 101 Building, Northwest Namie City, 99 Jinjihu Avenue, Suzhou Industrial Park, Jiangsu Province, 215000 Applicant after: SUZHOU FIRST ELEMENT NANO TECHNOLOGY CO.,LTD. Address before: Room 105 and 207, 101 Building, Northwest District of Suzhou Namie City, No. 99 Jinjihu Avenue, Wuzhong District Industrial Park, Suzhou City, Jiangsu Province, 215000 Applicant before: SUZHOU FIRST ELEMENT NANO TECHNOLOGY CO.,LTD. |
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Application publication date: 20190405 |