CN1541937A - Laser preparation and in-situ dispersion method for nanometer carbon granular material - Google Patents

Laser preparation and in-situ dispersion method for nanometer carbon granular material Download PDF

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Publication number
CN1541937A
CN1541937A CNA2003101050118A CN200310105011A CN1541937A CN 1541937 A CN1541937 A CN 1541937A CN A2003101050118 A CNA2003101050118 A CN A2003101050118A CN 200310105011 A CN200310105011 A CN 200310105011A CN 1541937 A CN1541937 A CN 1541937A
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China
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laser
liquid phase
nano carbon
distilled water
carbon
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CN1301213C (en
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刘常升
陈岁元
张滨
才庆魁
国玉军
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Northeastern University China
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Northeastern University China
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Abstract

The laser preparation and in-situ dispersion process of nano carbon grain material includes the following three steps: setting carbon containing target material in liquid phase; irradiating the carbon containing target material in liquid phase with laser beam; and solid-liquid separation to collect nano carbon grain. The said process is suitable for preparing amorphous carbon grain with size of 15-55 nm and realizing the in-situ dispersion and liquid phase collection and storing.

Description

The laser preparation and the original position dispersing method of nano carbon grain material
Technical field
The invention belongs to technical field of nano material, particularly preparation of a kind of laser of nano carbon grain material and original position dispersing method.
Background technology
Nano material is 21 century one of the most attractive research field, and nano carbon grain material is with a wide range of applications in fields such as electronics and chemical industry.At present, there are problems such as hard aggregation in the synthesis condition harshness of nano material between particle.The task of top priority is that to seek a kind of convenience feasible and be easy to control and collect the method for preparing nano carbon grain material of preservation.
Summary of the invention
Problem at prior art exists the invention provides a kind of carbon granule material of laser preparation of nano at normal temperatures and pressures and original position dispersing method, and this method is easy to collect, preserves and separates, and avoids hard aggregation between particle.
Principle of the present invention is that pulse laser sees through liquid phase irradiation graphite target, the local intensification rapidly of target reaches the vaporization temperature of graphite, make it distillation, simultaneously, the laser pulse shock action makes its part form high temperature and high pressure environment, generate the active plasma group of containing carbon atom, cluster, ion and electronics of high energy of carbon, the high-energy carbon forming core in the plasma group collides mutually, forms nano carbon particle and cancellation in liquid phase.In the cancellation process, the liquid phase vaporization, decomposition, the ionization that contact with plasma group become C, OH -, H +The isoreactivity group is stablized sp2 and sp3 hybridized orbital, and the control forming core is grown up.High-energy carbon particle in the plasma group is grown in liquid phase and is carried out energy exchange with it, and the corresponding product of generation and laser energy and reaction conditions also exists with the colloidal suspension state.Surface active agent composition in the liquid phase stops the generation of hard aggregation in situ in particulate generation and collision process, reduce the size of powder reuniting body.Nano carbon particle is preserved in liquid phase, can collect it easily by solid-liquid separation.
The present invention carries out according to the following steps
1. the carbon containing target is placed following one kind of liquid phase body, the liquid phase body has: the mixed solution that distilled water, ammoniacal liquor, tetrachloromethane, ethanol, acetone or distilled water and tensio-active agent are formed, make liquid level be higher than carbon containing target 1-2mm, the chemical reagent in the liquid phase body is chemical pure;
2. at normal temperatures and pressures, with the carbon containing target in the laser radiation liquid phase;
Irradiation time is 20-40 minute
Regulate laser focus 100-200mm
Spot diameter 0.5-2mm
Constantly change corrode point in the irradiation and splash into liquid phase, keep the liquid level in the synthesizer to be higher than target 1-2mm
3. solid-liquid separation is collected nano carbon particle.
Characteristics of the present invention are that laser type is the Nd:YAG solid statelaser, 1.06 microns of its wavelength, pulsewidth 5ms, frequency 4Hz, single pulse energy 0.4J.Preparation condition is a normal temperature and pressure.Target is a graphite etc.Liquid phase is the mixed solution of distilled water, ammoniacal liquor, tetrachloromethane, ethanol, acetone or distilled water and tensio-active agent, and tensio-active agent is an ethylene glycol etc., and the concentration of ethylene glycol is at 5-25%.
The present invention uses laser radiation to be positioned over carbon containing target in the liquid phase, interacts through laser and target, and physical-chemical reaction takes place at the solid-liquid interface place, generates nano carbon particle, and simultaneously, the tensio-active agent in the liquid phase makes it to obtain original position to be disperseed.Nano carbon particle is preserved in liquid phase, can collect it easily by solid-liquid separation, is suitable for preparing at normal temperatures and pressures the amorphous carbon particle of particle size between the 15-55 nanometer.
Embodiment
Example 1. is regulated laser apparatus, and focal length is 150mm, and spot diameter is 1mm, gets distilled water and graphite target places synthesizer, makes liquid level be higher than graphite target surface 1-2mm, starts laser apparatus, irradiation sample half an hour.Often change corrode point and splash into distilled water, keep liquid level to be higher than graphite target surface 1-2mm, the size minimum value of the nano carbon grain material of preparing is 26 nanometers, maximum value is 54 nanometers, and mean value is 40 nanometers, is non-crystalline state, have higher surface activity, be soft-agglomerated attitude.
Example 2. is regulated laser apparatus, and focal length is 150mm, and spot diameter is 1mm, gets ammoniacal liquor and graphite target places synthesizer, makes liquid level be higher than graphite target surface 1-2mm, starts laser apparatus, irradiation sample half an hour.Often change corrode point and splash into ammoniacal liquor, keep liquid level to be higher than graphite target surface 1-2mm, the size minimum value of the carbon nano-particle material of preparing is 16 nanometers, maximum value is 43 nanometers, and mean value is 29 nanometers, is non-crystalline state, have higher surface activity, be soft-agglomerated attitude.
Example 3. is regulated laser apparatus, and focal length is 150mm, and spot diameter is 1mm, gets tetrachloromethane and graphite target places synthesizer, makes liquid level be higher than graphite target surface 1-2mm, starts laser apparatus, irradiation sample half an hour.Often change corrode point and splash into tetrachloromethane, keep liquid level to be higher than graphite target surface 1-2mm, the size minimum value of the carbon nano-particle material of preparing is 15 nanometers, maximum value is 34 nanometers, and mean value is 22 nanometers, is non-crystalline state, have higher surface activity, be soft-agglomerated attitude.
Example 4. is regulated laser apparatus, and focal length is 150mm, and spot diameter is 1mm, gets ethanol and graphite target places synthesizer, makes liquid level be higher than graphite target surface 1-2mm, starts laser apparatus, irradiation sample half an hour.Often change corrode point and splash into ethanol, keep liquid level to be higher than graphite target surface 1-2mm, the size minimum value of the carbon nano-particle material of preparing is 41 nanometers, maximum value is 68 nanometers, and mean value is 52 nanometers, is non-crystalline state, have higher surface activity, be soft-agglomerated attitude.
Example 5. is regulated laser apparatus, and focal length is 150mm, and spot diameter is 1mm, gets acetone and graphite target places synthesizer, makes liquid level be higher than graphite target surface 1-2mm, starts laser apparatus, irradiation sample half an hour.Often change corrode point and splash into acetone, keep liquid level to be higher than graphite target surface 1-2mm, the size minimum value of the carbon nano-particle material of preparing is 26 nanometers, maximum value is 49 nanometers, and mean value is 38 nanometers, is non-crystalline state, have higher surface activity, be soft-agglomerated attitude.
Example 6. is regulated laser apparatus, and focal length is 150mm, and spot diameter is 1mm, gets distilled water, 10% ethylene glycol and graphite target place synthesizer, make liquid level be higher than graphite target surface 1-2mm, start laser apparatus, irradiation sample half an hour.Frequent conversion corrode point and splash into distilled water and 10% ethylene glycol mixture, keep liquid level to be higher than graphite target surface 1-2mm, the size minimum value of the carbon nano-particle material of preparing is 17 nanometers, maximum value is 39 nanometers, mean value is 29 nanometers, be non-crystalline state, particle agglomeration and overlapping phenomenon obviously alleviate, and it is all even tiny that particle size also is tending towards.

Claims (3)

1. the laser of a nano carbon grain material prepares and the original position dispersing method, it is characterized in that carrying out according to the following steps:
1. the carbon containing target is placed following one kind of liquid phase body, the liquid phase body has: the mixed solution of distilled water, ammoniacal liquor, tetrachloromethane, ethanol, acetone or distilled water and tensio-active agent makes liquid level be higher than carbon containing target 1-2mm;
2. at normal temperatures and pressures, with the carbon containing target in the laser radiation liquid phase;
Irradiation time is 20-40 minute
Regulate laser focus 100-200mm
Spot diameter 0.5-2mm
Constantly change corrode point in the irradiation and splash into liquid phase, keep the liquid level in the synthesizer to be higher than target 1-2mm;
3. solid-liquid separation is collected nano carbon particle.
2. preparation of the laser of nano carbon grain material as claimed in claim 1 and original position dispersing method is characterized in that used laser apparatus is the Nd:YAG solid statelaser, 1.06 microns of its wavelength, pulsewidth 5ms, frequency 4Hz, single pulse energy 0.4J.
3. the laser of nano carbon grain material as claimed in claim 1 preparation and original position dispersing method is characterized in that the tensio-active agent in the mixed solution of described distilled water and tensio-active agent is an ethylene glycol.
CNB2003101050118A 2003-11-06 2003-11-06 Laser preparation and in-situ dispersion method for nanometer carbon granular material Expired - Fee Related CN1301213C (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1313366C (en) * 2004-12-20 2007-05-02 天津大学 Method for synthesizing nano diamond by laser bombarding carbon powder
CN107381548A (en) * 2017-07-31 2017-11-24 江苏大学 A kind of laser quick in situ prepares the apparatus and method with transfer large-area graphene
CN107383595A (en) * 2017-07-17 2017-11-24 厦门稀土材料研究所 A kind of anti-ultraviolet polypropene composition and its polypropylene and polypropylene film of preparation
CN108865123A (en) * 2018-06-06 2018-11-23 国家纳米科学中心 A kind of fluorescent carbon nano-particles and its preparation method and application

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100484870C (en) * 2001-10-16 2009-05-06 福建师范大学 Laser impact process of synthesizing diamond nanometer bead (sol) continuously

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1313366C (en) * 2004-12-20 2007-05-02 天津大学 Method for synthesizing nano diamond by laser bombarding carbon powder
CN107383595A (en) * 2017-07-17 2017-11-24 厦门稀土材料研究所 A kind of anti-ultraviolet polypropene composition and its polypropylene and polypropylene film of preparation
CN107383595B (en) * 2017-07-17 2019-10-01 厦门稀土材料研究所 A kind of anti-ultraviolet polypropene composition and its polypropylene and polypropylene film of preparation
CN107381548A (en) * 2017-07-31 2017-11-24 江苏大学 A kind of laser quick in situ prepares the apparatus and method with transfer large-area graphene
CN108865123A (en) * 2018-06-06 2018-11-23 国家纳米科学中心 A kind of fluorescent carbon nano-particles and its preparation method and application

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