CN109650380B - Method for preparing carbon nano onion by dry friction in vacuum environment - Google Patents

Method for preparing carbon nano onion by dry friction in vacuum environment Download PDF

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CN109650380B
CN109650380B CN201910051920.9A CN201910051920A CN109650380B CN 109650380 B CN109650380 B CN 109650380B CN 201910051920 A CN201910051920 A CN 201910051920A CN 109650380 B CN109650380 B CN 109650380B
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friction
vacuum environment
carbon nano
disc
polyethylene
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CN109650380A (en
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张俊彦
曹忠跃
梁爱民
王富国
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Lanzhou Institute of Chemical Physics LICP of CAS
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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
    • C01B32/18—Nanoonions; Nanoscrolls; Nanohorns; Nanocones; Nanowalls
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM

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  • Condensed Matter Physics & Semiconductors (AREA)
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  • Carbon And Carbon Compounds (AREA)

Abstract

The invention relates to a method for preparing carbon nano onion by dry friction in a vacuum environment, which comprises the steps of fixing a hydrogen-containing carbon film or polyethylene on a disc of a friction tester in the vacuum environment, carrying out sliding friction with a ceramic ball by rotating the disc under the condition that the contact positive pressure stress is not less than 0.5 GPa, and collecting a substance formed on the surface of the ceramic ball when the friction coefficient is not more than 0.01, wherein the substance is the carbon nano onion. The invention adopts dry friction technology, takes the hydrogen-containing carbon film or polyethylene and ceramic balls as friction pairs, and performs opposite grinding in a vacuum environment to form CNOs on a friction interface, and has the characteristics of simple equipment, low energy consumption, no need of harsh conditions such as high temperature, catalyst and the like, capability of continuously and stably working for a long time, realization of industrial production and the like.

Description

Method for preparing carbon nano onion by dry friction in vacuum environment
Technical Field
The invention relates to the technical field of zero-dimensional carbon nano materials, in particular to a method for preparing carbon nano onions by dry friction in a vacuum environment.
Background
Carbon Nano Onions (CNOs), also known as onion nanostructured carbon, are novel zero-dimensional carbon nanomaterials consisting of quasi-spherical or polyhedral graphite-like shells with a nanostructure similar to that of onion concentric circles. Due to the closed stable structure, the large specific surface area and the high thermal stability, the material has wide potential application value in the fields of catalysis, friction, supercapacitors, electromagnetic shielding and the like, and is widely concerned by technologists. In recent 30 years, the preparation method mainly focuses on the aspects of arc discharge, electron beam irradiation, plasma method, nano-diamond vacuum heat treatment, organic metal polymer pyrolysis method, laser irradiation method and the like. However, most of these methods require high energy (for example, the thermal treatment of nanodiamonds generally requires high temperature conditions exceeding 1400 ℃ and maintained in a vacuum environment) or special catalysts (for example, the CVD method generally requires Ni/Al, Cu, etc. as a catalyst while requiring high temperature conditions exceeding 500 ℃). Therefore, new techniques and methods are needed to be developed to easily prepare high-quality CNOs to meet the scientific research and application deficiencies.
Recently, several new methods for preparing CNOs have been successively reported, such as preparing CNOs by hydrothermal reaction (using water as reaction medium, containing citrate, selected from Li)+、Na+、K+、Ca2+、Mg2+、Ba2+、Al3+Can realize the preparation of CNOs at the temperature of more than or equal to 140 ℃, and the preparation of water-soluble CNOs by the concentrated nitric acid treatment of carbonized wood waste, and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a simple and environment-friendly method for preparing carbon nano onions by dry friction in a vacuum environment.
In order to solve the problems, the method for preparing the carbon nano onion by dry friction in the vacuum environment is characterized by comprising the following steps: the method comprises the steps of fixing a hydrogen-containing carbon film or polyethylene on a disc of a friction tester in a vacuum environment, carrying out sliding friction with a ceramic ball by rotating the disc under the condition that the contact positive pressure stress is more than or equal to 0.5 GPa, and collecting a substance formed on the surface of the ceramic ball when the friction coefficient is less than or equal to 0.01, wherein the substance is the carbon nano onion.
The vacuum environment refers to that the vacuum degree is less than or equal to 1.0 multiplied by 10-3Pa。
The rotating speed of the disc is 50-200 revolutions per minute.
Compared with the prior art, the invention has the following advantages:
1. the invention adopts dry friction technology, takes the hydrogen-containing carbon film or polyethylene and ceramic balls as friction pairs, and performs opposite grinding in a vacuum environment to form CNOs on a friction interface, and has the characteristics of simple equipment, low energy consumption, no need of harsh conditions such as high temperature, catalyst and the like, capability of continuously and stably working for a long time, realization of industrial production and the like.
2. The CNOs obtained by the present invention were characterized by a Transmission Electron Microscope (TEM) and the like (see fig. 1). The result shows that the newly formed substance on the surface of the ceramic dual-sphere consists of carbon nanoparticles (the particle size is distributed in the range of 5-100 nm); high resolution images confirm that the carbon nanoparticles present the structural characteristics of nano-onion (the spacing between graphene shells is about 0.34 nm); the corresponding EDX energy spectrum shows that the nano-particles have no other impurities except carbon.
3. The method is simple and easy to implement and has good repeatability.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Fig. 1 shows the structural characteristics of carbon nano onion particles prepared by the present invention. Wherein: (a) low power transmission electron microscope images; (b) high resolution transmission electron microscope images; (c) EDX spectra of the respective regions.
Detailed Description
Example 1A method for preparing carbon nano-onions by dry friction in a vacuum environment, in which a hydrogen-containing carbon film with a smooth surface is fixed on a sample stage (disk) of a UMT friction tester, and Al with a diameter of 5 mm is selected2O3The ceramic balls are used as dual balls; sealing the vacuum container in a vacuum chamber, starting to vacuumize until the vacuum is not more than 1.0 × 10-3And when Pa is higher than Pa, setting normal loading to be more than or equal to 1N (contact stress to be more than or equal to 0.5 GPa), setting the rotating speed of the disc to be 50-200 revolutions per minute, performing sliding friction through the rotating disc, and collecting substances formed on the surface of the ceramic ball after the friction coefficient is less than or equal to 0.01 and the disc is stabilized for a period of time, wherein the substances are carbon nano onions.
Example 2A method for preparing carbon nano-onions by dry friction in a vacuum environment, in which polyethylene with a smooth surface is fixed on a sample stage (disk) of a CSM friction tester, ZrO with a diameter of 5 mm is selected2The ceramic balls are used as dual balls; sealing the vacuum container in a vacuum chamber, starting to vacuumize until the vacuum is not more than 1.0 × 10-3When Pa is needed, setting the normal loading to be more than or equal to 1N (the contact stress is more than or equal to 0.5 GPa), setting the rotating speed of the disc to be 50-200 r/min, performing sliding friction through the rotating disc, and stabilizing the disc until the friction coefficient is less than or equal to 0.01And collecting the substance formed on the surface of the ceramic ball after a period of time, wherein the substance is the carbon nano onion.

Claims (1)

1. A method for preparing carbon nano onion by dry friction in a vacuum environment is characterized by comprising the following steps: the method comprises the steps that under a vacuum environment, polyethylene with a smooth surface is fixed on a disc of a friction tester, the polyethylene and a ceramic ball are subjected to sliding friction through rotating the disc under the condition that the contact positive pressure stress is larger than or equal to 0.5 GPa, and when the friction coefficient is smaller than or equal to 0.01, a substance formed on the surface of the ceramic ball is collected, wherein the substance is the carbon nano onion; the vacuum environment refers to that the vacuum degree is less than or equal to 1.0 multiplied by 10-3Pa; the rotating speed of the disc is 50-200 revolutions per minute.
CN201910051920.9A 2019-01-21 2019-01-21 Method for preparing carbon nano onion by dry friction in vacuum environment Active CN109650380B (en)

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Publication number Priority date Publication date Assignee Title
CN109867275B (en) * 2019-03-11 2020-10-30 西安石油大学 Method for preparing carbon nano onion by vacuum ball milling
CN113800519B (en) * 2021-10-19 2022-11-25 中国科学院兰州化学物理研究所 Preparation method and application of MXene-based composite lubricating coating
CN115283667B (en) * 2022-06-29 2024-02-23 燕山大学 Preparation method for synthesizing onion carbon in situ by laser

Citations (4)

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WO2017104822A1 (en) * 2015-12-18 2017-06-22 日本アイ・ティ・エフ株式会社 Coating film, manufacturing method therefor, and pvd apparatus
CN108220910A (en) * 2017-12-18 2018-06-29 中国科学院兰州化学物理研究所 A kind of preparation method of in-situ preparation nano-onions carbon
CN108220908A (en) * 2017-12-18 2018-06-29 中国科学院兰州化学物理研究所 A kind of method that frictional interface is formed in situ graphene and onion realizes superslide
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WO2017104822A1 (en) * 2015-12-18 2017-06-22 日本アイ・ティ・エフ株式会社 Coating film, manufacturing method therefor, and pvd apparatus
CN108220910A (en) * 2017-12-18 2018-06-29 中国科学院兰州化学物理研究所 A kind of preparation method of in-situ preparation nano-onions carbon
CN108220908A (en) * 2017-12-18 2018-06-29 中国科学院兰州化学物理研究所 A kind of method that frictional interface is formed in situ graphene and onion realizes superslide
CN108529598A (en) * 2018-06-20 2018-09-14 北京师范大学 A kind of preparation method of carbon nano-onions

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"Perspectives of friction mechanism of a-C:H film in vacuum concerning the onion-like carbon transformation at the sliding interface";Hui Song et al.;《RSC Advances》;20141219;第8904-911页 *

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