CN1116255C - Nanometer microparticle catalytic onion-like fullerene and its preparation - Google Patents
Nanometer microparticle catalytic onion-like fullerene and its preparation Download PDFInfo
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- CN1116255C CN1116255C CN 00101463 CN00101463A CN1116255C CN 1116255 C CN1116255 C CN 1116255C CN 00101463 CN00101463 CN 00101463 CN 00101463 A CN00101463 A CN 00101463A CN 1116255 C CN1116255 C CN 1116255C
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Abstract
The present invention relates to a nanometer particle catalyzed onion-shaped fullerene and preparation which belongs to the technical field of new material synthesizing and processing engineering. Coal is used as raw material, and an irradiation technique of high energy rays is used; the present invention discloses a new fullerene structure and a preparation technique. The onion-shaped fullerene of the present invention is a lamellar compound whose metal atoms are regularly distributed among onion-shaped layers; the onion-shaped fullerene is composed of monocaryon fullerene and multikaryon fullerene, and a little of monocaryon fullerene can be joined into large multikaryon fullerene; a little of onion-shaped fullerene is joined or stacked to form a fullerene thin film with a mutual twin crystal structure; the onion-shaped fullerene can be formed by the migration catalysis of activated nanometer particles or nanometer particles. The onion-shaped fullerene is mainly used as functional material.
Description
Onion-like fullerene that nanometer microparticle catalytic of the present invention forms and preparation belong to the synthetic and processing engineering technology category of novel material, relate generally to fields such as Materials science such as nano material, carbon material, information material, coal science, crystallography.
At present, it is a lot of to prepare the method for onion-like fullerene.Wherein, employing can obtain to have onion-like fullerene new function material structure successive, film like or patterning by the method for metallic nano-particle catalysis amorphous carbon membrane prepare onion-like fullerene under electron beam irradiation, this method technology simple possible, high, the good reproducibility of stability, and can control the nucleation site, growth process, engagement state etc. of onion-like fullerene well.But need in the preparation metallic nano-particle is configured on the amorphous carbon film, because the unstable of amorphous carbon film makes that the success ratio of preparation process is not very high.In addition, the preparation cost of amorphous carbon film and metallic nano-particle is higher, has brought difficulty for magnanimity prepares the onion-like fullerene material.
The onion-like fullerene that nanometer microparticle catalytic of the present invention forms and the purpose of preparation are to utilize cheap resource---coal, adopt the irradiation technique of energy beam, disclose a kind of onion-like fullerene structure and preparation technology who is formed by nanometer microparticle catalytic.
The onion-like fullerene that nanometer microparticle catalytic of the present invention forms is by with C
60The shell multilayer big or small for the difference of core coats the concentric spherical shell that the interval that forms is about 0.3nm-0.5nm, and single or multiple metallic nano-particles are inclusive in the onion-like fullerene cavity.It is characterized in that: A. is the lamellar compound that a kind of atoms metal regular distribution forms between onion shape layer and layer; B. form by monokaryon soccerballene and multinuclear soccerballene and several monokaryon soccerballene can to engage be the onion-like fullerene of the huge soccerballene of multinuclear; C. be that a kind of a plurality of onion-like fullerene engages or pile up the fullerene thin film with mutual twin structure of formation; D. onion-like fullerene both can be formed by the activated nanometer microparticle catalytic, also can be formed by nanoparticle catalysis in transition process.
The method for preparing the onion-like fullerene of above-mentioned nanometer microparticle catalytic formation is characterized in that utilizing coal; with the basis of nanoparticle as the soccerballene forming core; coal particles is mixed with nanoparticle; form the mixture of nanoparticle and coal; shine this mixture with energy beam then; under the acting in conjunction of nanoparticle and energy beam, coal is converted into onion-like fullerene at low temperatures.The step of its concrete preparation process is: A. carries out fine purifiation, grinding, ultrasonic dispersing to coal, obtains the coal particles that granularity is 100nm-500nm; Gac can obtain by control temperature of combustion and atmosphere, and it is pulverized and the ultrasonic wave grinding, obtains the activated carbon granule that granularity is 50nm-300nm; B. by Ar
+Ion arc sputtering method or excitation electron absorption process obtain metallic nano-particle or the metal oxide nanoparticles of single or multiple 1nm-100nm; C. coal particles or activated carbon granule are mixed with nanoparticle, obtain the mixture of coal particles or activated carbon granule and nanoparticle; D. the above-mentioned mixture of energy beam that is enough to activate coal particles or activated carbon granule with exposure intensity carries out irradiation, adopts protective atmosphere during irradiation, through behind the 50s, generates the multinuclear onion-like fullerene; E. the onion-like fullerene that has generated is proceeded the irradiation of energy beam, nanoparticle is moved out from the onion-like fullerene shell gradually, the monokaryon onion-like fullerene is bonded into the multinuclear onion-like fullerene, behind the irradiation 1000s, onion-like fullerene engages or is piled into the fullerene thin film with mutual twin structure.
The preparation method of the onion-like fullerene that above-mentioned nanometer microparticle catalytic forms is characterized in that described nanoparticle comprises pure metal nanoparticle Al, Cu, Mn, Mo, Ni, Pt, Fe, Co, La, W and metal oxide nanoparticles LaO, Al
2O
3, Mo
2O
5, TiO
3
The preparation method of the onion-like fullerene that above-mentioned nanometer microparticle catalytic forms is characterized in that described coal particles or activated carbon granule and the hybrid mode of nanoparticle comprise that coal particles or activated carbon granule engage with nanoparticle, coal particles or activated carbon granule with the nanoparticle heap bury, regular dispose etc. of coal particles or activated carbon granule and nanoparticle see accompanying drawing 1;
The preparation method of the onion-like fullerene that above-mentioned nanometer microparticle catalytic forms is characterized in that described energetic ray is electron beam, ionic fluid etc., and exposure intensity is 10
19E/cm
2S ∽ 10
23E/cm
2S, irradiation time is 50s-2000s, the atmosphere during irradiation is 10
-4Vacuum, N that Pa is above
2, the Ar rare gas element, its effect is the activated nano particulate, promote onion-like fullerene forming core, grow up.
Onion-like fullerene and preparation that nanometer microparticle catalytic of the present invention forms; its advantage is to utilize cheap coal resources; allocation position, size, kind according to nanoparticle and coal particles or activated carbon granule; processing parameters such as atmosphere when the exposure intensity of adjustment energetic ray, irradiation time, irradiation; nucleation site, growth process and the engagement state of control onion-like fullerene, the onion-like fullerene material that obtains having the performance that requires.This provides for the function of utilizing coal resources more widely, more effectively carrying out coal transforms may.
The onion-like fullerene of onion-like fullerene that nanometer microparticle catalytic of the present invention forms and preparation gained, its purposes is to utilize the engagement characteristics of onion-like fullerene, electroconductibility, quantum mechanical effects (quantum well, little can the band etc.) etc. key property, be used as the electronic component that property requires, filter element, the material of Device elements such as senser element, superconducting material, biomaterial, medical material, the new pattern laser material, nonlinear optical material, information storage material, photoelectric material, catalystic material, waste water, new function materials such as waste-gas cleaning material, range of application is very wide, and application prospect is very good.
Description of drawings: [accompanying drawing 1] coal particles or activated carbon granule engage the onion-like fullerene thin-film material that forms with a plurality of onion-like fullerenes of onion-like fullerene synoptic diagram [accompanying drawing 4] that nanoparticle hybrid mode synoptic diagram [accompanying drawing 2] lamellar compound synoptic diagram [accompanying drawing 3] nanoparticle is contained
Synoptic diagram nomenclature: the multinuclear onion-like fullerene film that (1) coal particles (2) activated carbon granule (3) nanoparticle (4) lamellar compound (5) nanoparticle moving out from the onion-like fullerene shell (6) monokaryon onion-like fullerene forms
Embodiment 1
Placing micro-granularity on the little aperture plate of metal is the coal particles of 500nm and the Al particulate that diameter is 100nm, be placed on the room temperature Stage microscope in the vacuum chamber, with acceleration voltage 3.5Kv, the little aperture plate of the ar-ion beam of beam current 0.3mA irradiation metal, the atmosphere during irradiation is 1 * 10
-3The vacuum of Pa (containing argon gas).Under the irradiation of ar-ion beam, coal particles can with
AlParticulate engages, and also Al particulate heap can be buried, and obtains the mixture of coal particles and Al particulate.This mixture is moved on the room temperature Stage microscope in the JEM-2010 electron microscope vacuum chamber, 1 * 10
-3Under the vacuum condition of Pa, be 1 * 10 with intensity
19E/cm
2.s electron beam shines mixture from the little aperture plate of metal top, simultaneously it is carried out TEM and dynamic observes.300s begins to occur soccerballene, and soccerballene has two kinds of monokaryon and multinuclears, and this is that a kind of lamellar compound is seen accompanying drawing 2.Coal particles is converted into onion-like fullerene fully behind the 900s, and nanoparticle is proceeded irradiation from the onion shape gradually, and behind the 1500s, onion-like fullerene couples together, and formation onion shape richness is reined in film alkene material and seen accompanying drawing 4.
Embodiment 2
Placing micro-granularity on the little aperture plate of metal is the coal particles of 100nm, on coal particles, generate the Pt nanoparticle that granularity is 1nm by the argon ion sputtering technology, be placed on then on the room temperature Stage microscope in the vacuum chamber, with acceleration voltage 3.5Kv, the little aperture plate of ar-ion beam irradiation metal of beam current 0.25mA, the atmosphere during irradiation is 1 * 10
-3The vacuum of Pa (containing argon gas).Under the irradiation of ar-ion beam, coal particles and Pt particulate engage or Pt particulate heap are buried, and obtain the mixture of coal particles and Pt particulate.This mixture is moved on the room temperature Stage microscope in the JEM-2010 electron microscope vacuum chamber, 1 * 10
-3Under the vacuum condition of Pa, be 1 * 10 with intensity
23E/cm
2.s electron beam shines mixture from the little aperture plate of metal top, simultaneously it is carried out TEM and dynamic observes.100s begins to occur soccerballene, and coal particles is converted into onion-like fullerene fully behind the 700s.Proceed irradiation, behind the 1100s, onion-like fullerene couples together, and forms the onion-like fullerene thin-film material.
Placing micro-granularity on the little aperture plate of metal is the activated carbon granule of 50nm and the Al particulate that diameter is 20nm, be placed on the room temperature Stage microscope in the vacuum chamber, with acceleration voltage 3.5Kv, the little aperture plate of the ar-ion beam of beam current 0.3mA irradiation metal, the atmosphere during irradiation is 1 * 10
-3The vacuum of Pa (containing argon gas).Under the irradiation of ar-ion beam, activated carbon granule can engage with the Al particulate, also Al particulate heap can be buried, and obtains the mixture of activated carbon granule and Al particulate.This mixture is moved on the room temperature Stage microscope in the JEM-2010 electron microscope vacuum chamber, 1 * 10
-3Under the vacuum condition of Pa, be 1 * 10 with intensity
19E/cm
2.s electron beam shines mixture from the little aperture plate of metal top, simultaneously it is carried out TEM and dynamic observes.100s begins to occur soccerballene, and activated carbon granule is converted into onion-like fullerene fully behind the 750s.Proceed irradiation, behind the 1000s, onion-like fullerene couples together, and forms the onion-like fullerene material.
Placing micro-granularity on the little aperture plate of metal is the activated carbon granule of 300nm and the Pt particulate that diameter is 6nm, be placed on the room temperature Stage microscope in the vacuum chamber, with acceleration voltage 3.0Kv, the little aperture plate of the ar-ion beam of beam current 0.25mA irradiation metal, the atmosphere during irradiation is 1 * 10
-3The vacuum of Pa (containing argon gas).Under the irradiation of ar-ion beam, activated carbon granule can engage with the Pt particulate, also Pt particulate heap can be buried, and obtains the mixture of activated carbon granule and Pt particulate.This mixture is moved on the room temperature Stage microscope in the JEM-2010 electron microscope vacuum chamber, 1 * 10
-3Under the vacuum condition of Pa, be 1 * 10 with intensity
23E/cm
2.s electron beam shines mixture from the little aperture plate of metal top, simultaneously it is carried out TEM and dynamic observes.150s begins to occur soccerballene, and activated carbon granule is converted into onion-like fullerene fully behind the 800s.Proceed irradiation, behind the 1300s, onion-like fullerene couples together, and forms the onion-like fullerene material.
Claims (5)
1. the onion-like fullerene that forms of nanometer microparticle catalytic is by with C
60The shell multilayer big or small for the difference of core coats the concentric spherical shell that the interval that forms is about 0.3nm-0.5nm, and single or multiple metallic nano-particles are inclusive in the onion-like fullerene cavity, it is characterized in that:
A. be the lamellar compound that a kind of atoms metal regular distribution forms between onion shape layer and layer;
B. form by monokaryon soccerballene and multinuclear soccerballene and several monokaryon soccerballene can to engage be the onion-like fullerene of the huge soccerballene of multinuclear;
C. be that a kind of a plurality of onion-like fullerene engages or pile up the fullerene thin film with mutual twin structure of formation;
D. onion-like fullerene both can be formed by the activated nanometer microparticle catalytic, also can be formed by nanoparticle catalysis in transition process.
2. the method for preparing the described onion-like fullerene of claim 1; it is characterized in that utilizing coal; with the basis of nanoparticle as the soccerballene forming core; coal particles is mixed with nanoparticle; form the mixture of coal particles and nanoparticle, shine this mixture with energy beam then, under the acting in conjunction of nanoparticle and energy beam; coal generates onion-like fullerene at low temperatures, and the step of its concrete preparation process is:
A. coal is carried out fine purifiation, grinding, ultrasonic dispersing, obtain the coal particles that granularity is 100nm-500nm, gac can obtain by control temperature of combustion and atmosphere, and it is pulverized and the ultrasonic wave grinding, obtains the activated carbon granule that granularity is 50nm-300nm;
B. by Ar
+Ion arc sputtering method or excitation electron absorption process obtain metallic nano-particle or the metal oxide nanoparticles of single or multiple 1nm-100nm;
C. coal particles or activated carbon granule are mixed with nanoparticle, obtain the mixture of coal particles or activated carbon granule and nanoparticle;
D. the energy beam that is enough to activate coal particles or activated carbon granule with exposure intensity carries out irradiation to above-mentioned mixture, adopts protective atmosphere during irradiation, through after the 50s, generates the multinuclear onion-like fullerene;
E. the onion-like fullerene that has generated is proceeded the irradiation of energy beam, nanoparticle is moved out from the onion-like fullerene shell gradually, the monokaryon onion-like fullerene is bonded into the multinuclear onion-like fullerene, behind the 1000s, onion-like fullerene engages or is piled into the fullerene thin film with mutual twin structure.
3. according to the preparation method of the described onion-like fullerene of claim 2, it is characterized in that described nanoparticle comprises pure metal nanoparticle Al, Cu, Mn, Mo, Ni, Pt, Fe, Co, La, W and metal oxide nanoparticles LaO, Al
2O
3, Mo
2O
5, TiO
3
4. according to the preparation method of the described onion-like fullerene of claim 2, it is characterized in that described coal particles or activated carbon granule and the hybrid mode of nanoparticle comprise that coal particles or activated carbon granule engage with nanoparticle, coal particles or activated carbon granule with the nanoparticle heap bury, coal particles or activated carbon granule dispose with the nanoparticle rule.
5. according to the preparation method of the described onion-like fullerene of claim 2, it is characterized in that described energy beam is electron beam, ionic fluid, exposure intensity is 10
19E/cm
2S-10
23E/cm
2.s, irradiation time is 50s-2000s, and the protective atmosphere during irradiation is 10
-4Vacuum, N that Pa is above
2, the Ar rare gas element.
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| CN 00101463 CN1116255C (en) | 2000-01-20 | 2000-01-20 | Nanometer microparticle catalytic onion-like fullerene and its preparation |
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| CN1116255C true CN1116255C (en) | 2003-07-30 |
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| CN1318294C (en) * | 2005-05-10 | 2007-05-30 | 太原理工大学 | Catalytic pyrolysis method for preparing metal particle-encapsulating onion-like Fullerene |
| CN102060285A (en) * | 2010-11-03 | 2011-05-18 | 天津大学 | Method for preparing carbon nano-onion by chemical vapor deposition of Fe-Y catalyst on Cu carrier |
| CN115283667B (en) * | 2022-06-29 | 2024-02-23 | 燕山大学 | Preparation method for synthesizing onion carbon in situ by laser |
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