CN109179420B - B4Preparation method of C nanobelt - Google Patents

B4Preparation method of C nanobelt Download PDF

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CN109179420B
CN109179420B CN201811240955.9A CN201811240955A CN109179420B CN 109179420 B CN109179420 B CN 109179420B CN 201811240955 A CN201811240955 A CN 201811240955A CN 109179420 B CN109179420 B CN 109179420B
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nanobelt
preparation
temperature
sintering
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CN109179420A (en
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钟博
王猛
夏龙
张涛
王春雨
王华涛
覃春林
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Weihai Yunshan Technology Co ltd
Harbin Institute of Technology Weihai
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Harbin Institute of Technology Weihai
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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
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/991—Boron carbide
    • 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
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
    • 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
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

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  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Organic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
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Abstract

The invention provides a4The preparation method of the C nanobelt comprises the following steps of 1, mixing: uniformly dispersing the polyaminoborane and the polycarbosilane into tetrahydrofuran to obtain a mixture; step 2, drying: drying the mixture obtained in the step 1 at the temperature of 50-60 ℃; step 3, grinding: grinding the dried mixture into precursor powder; step 4, sintering and material taking: sintering the precursor powder in a protective gas environment, keeping the temperature for 0.5-1.5 h in the protective gas environment when the sintering temperature reaches 1400 ℃, and preparing B by a vapor deposition method4C nanobelt, and then when the temperature is reduced, obtaining B4C nanobelts. The nanobelt prepared by the above preparation method is a single crystal B having a uniform width and thickness4The preparation method can simplify the process flow and shorten the preparation time of the C nanobelt4The C nanobelt still keeps higher purity and conversion rate, so that the production cost is obviously reduced, and the C nanobelt has a wider application prospect.

Description

B4Preparation method of C nanobelt
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a B4Preparation of C nanobeltsA method.
Background
Boron carbide is one of the most attractive non-oxide materials and has important application in high-tech fields such as civil use, aviation, military, nuclear industry and the like. It is a rhombohedral structure whose structure can be described as a cubic primitive lattice extending in the direction of the spatial diagonal, forming a fairly regular twenty faces on each corner. Boron carbide has many excellent physicochemical properties due to its special crystal structure, and its main properties include low density, high hardness (second to diamond and cubic boron nitride), high melting point and high temperature wear resistance, low thermal expansion coefficient, excellent thermoelectric properties, strong thermal neutron absorption capacity, good chemical stability, etc. Boron carbide is therefore widely used for metal polishing and cutting, lightweight armor and high temperature thermoelectric conversion applications. Meanwhile, boron carbide is also a p-type semiconductor and is considered as a promising high-temperature electronic device material.
In recent years, one-dimensional nanomaterials have attracted great attention, and one-dimensional boron carbide nanostructures with different morphologies, including nanowires, nanobelts, and nanorods, have been reported. There is still a lack of an effective method for producing boron carbide nanoribbons.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a B4A preparation method of C nanobelt, so that B can be prepared on the premise of simplifying the process flow and shortening the preparation time4The C nanobelt still maintains higher purity and conversion rate.
In order to achieve the above purpose, the invention provides a B4The preparation method of the C nanobelt comprises the following steps of:
step 1, mixing materials: uniformly dispersing polyaminoborane and polycarbosilane into tetrahydrofuran to obtain a mixture, wherein the molar percentage of the polyaminoborane is 30-40%, and the molar percentage of the polycarbosilane is 60-70%;
step 2, drying: drying the mixture obtained in the step 1 at the temperature of 50-60 ℃;
step 3, grinding: grinding the dried mixture into precursor powder;
step 4, sintering and material taking: sintering the precursor powder in a protective gas environment, keeping the temperature for 0.5 to 1.5 hours in the protective gas environment when the sintering temperature reaches 1400 ℃, namely keeping the temperature for 0.5 to 1.5 hours, and preparing B by a vapor deposition method4C nanobelt, and then when the temperature is reduced, obtaining B4C nanobelts.
Preferably, in the step 1, the polyaminoborane and the polycarbosilane are uniformly dispersed in the tetrahydrofuran under the combined action of ultrasonic oscillation and mechanical stirring.
Preferably, in the step 4, the incubation time is 1 hour.
Preferably, in the step 4, the precursor powder obtained in the step 3 is placed in a container, and the container is placed in a furnace to be sintered in an argon or nitrogen environment.
Preferably, a high temperature tube furnace is used.
The scheme of the invention has the beneficial effect that the invention passes through the B4C preparation method of nanobelt the nanobelt prepared by the method is a single crystal B with uniform width and thickness4C nanoribbon, said B4The length of C nanoribbon is in the range of hundreds of micrometers to several millimeters, and B4C nanoribbons are very thin, ranging in width from 500nm to 3 μm, each B4C nanoribbons having uniform width and thickness along their entire length, B4The surface of the C nanobelt was neat, there were no dislocations and defects, and no droplets were observed on the tip of the nanobelt. B according to the invention4The preparation method of the C nanobelt can simplify the process flow and shorten the preparation time of the B nanobelt4The C nanobelt still keeps higher purity and conversion rate, so that the production cost is obviously reduced, and the C nanobelt has a wider application prospect.
Drawings
FIGS. 1(a), (B), (c) and (d) show B at different magnifications4SEM image of C nanobelts.
FIG. 2(a) shows B4Typical low power of C nanoribbonA TEM image; FIG. 2(B) shows B4C nano-band high-resolution TEM image; FIG. 2(c) shows B4SAED pattern of C nanobelts; FIG. 2(d) shows measurement B4(101) interplanar spacing pattern of C nanoribbons.
FIG. 3 shows B prepared4EDX analysis of C nanobelts.
FIG. 4 shows B prepared4Microscopic raman spectrum of C nanobelt.
Detailed Description
The present invention will be further described with reference to the following examples.
B according to the invention4The preparation method of the C nanobelt comprises the following steps of:
step 1, mixing materials: uniformly dispersing the polyaminoborane and the polycarbosilane into tetrahydrofuran to obtain a mixture, wherein the molar percentage of the polyaminoborane is 30-40%, and the molar percentage of the polycarbosilane is 60-70%. Specifically, the polyaminoborane and the polycarbosilane can be uniformly dispersed in the tetrahydrofuran under the combined action of ultrasonic oscillation and mechanical stirring. The polyaminoborane can be obtained by heating commercially available or self-prepared ammonia borane; the polycarbosilane and tetrahydrofuran are commercially available analytical grade.
Step 2, drying: and (3) drying the mixture obtained in the step (1), wherein the drying temperature is 50-60 ℃.
Step 3, grinding: the dried mixture was ground to a precursor powder.
Step 4, sintering and material taking: sintering the precursor powder in a protective gas environment, keeping the temperature for 0.5 to 1.5 hours in the protective gas environment when the sintering temperature reaches 1400 ℃, namely keeping the temperature for 0.5 to 1.5 hours, wherein 1 hour is the best, and preparing B by a vapor deposition method4C nanobelt, and then when the temperature is reduced, obtaining B4C nanobelts. The specific sintering and material taking process is as follows: the precursor powder obtained in step 3 is placed in a container, in this embodiment, a box made of graphite paper is used as the container, and the container is placed in a furnace to be sintered in an argon or nitrogen environment, so that the sintering is performed in the furnaceIn an embodiment, a high temperature tube furnace may be used. No catalyst is used in the chemical vapor deposition process in this step.
By means of B in accordance with the invention4C preparation method of nanobelt the nanobelt prepared by the method is a single crystal B with uniform width and thickness4C nanoribbon, said B4The length of C nanoribbon is in the range of hundreds of micrometers to several millimeters, and B4C nanoribbons are very thin, ranging in width from 500nm to 3 μm, each B4C nanoribbons having uniform width and thickness along their entire length, B4The surface of the C nanobelt was neat, there were no dislocations and defects, and no droplets were observed on the tip of the nanobelt. B according to the invention4The preparation method of the C nanobelt can simplify the process flow and shorten the preparation time of the B nanobelt4The C nanobelt still keeps higher purity and conversion rate, so that the production cost is obviously reduced, and the C nanobelt has a wider application prospect.

Claims (5)

1. B4The preparation method of the C nanobelt is characterized by comprising the following steps: the method comprises the following steps:
step 1, mixing materials: uniformly dispersing polyaminoborane and polycarbosilane into tetrahydrofuran to obtain a mixture, wherein the molar percentage of the polyaminoborane is 30-40%, and the molar percentage of the polycarbosilane is 60-70%;
step 2, drying: drying the mixture obtained in the step 1 at the temperature of 50-60 ℃;
step 3, grinding: grinding the dried mixture into precursor powder;
step 4, sintering and material taking: sintering the precursor powder in a protective gas environment, keeping the temperature for 0.5 to 1.5 hours in the protective gas environment when the sintering temperature reaches 1400 ℃, namely keeping the temperature for 0.5 to 1.5 hours, and preparing B by a vapor deposition method4C nanobelt, and then when the temperature is reduced, obtaining B4C nanobelts.
2. B according to claim 14The preparation method of the C nanobelt is characterized by comprising the following steps: in the step 1, the polyaminoborane and the polycarbosilane are uniformly dispersed into the tetrahydrofuran under the combined action of ultrasonic oscillation and mechanical stirring.
3. B according to claim 14The preparation method of the C nanobelt is characterized by comprising the following steps: in the step 4, the heat preservation time is 1 h.
4. B according to claim 14The preparation method of the C nanobelt is characterized by comprising the following steps: in the step 4, the precursor powder obtained in the step 3 is placed in a container, and the container is placed in a furnace to be sintered in an argon or nitrogen environment.
5. B according to claim 44The preparation method of the C nanobelt is characterized by comprising the following steps: a high temperature tube furnace is used.
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CN110511748A (en) * 2019-08-07 2019-11-29 陕西师范大学 A kind of preparation method of fluorescence boron carbide nanobelt
CN112321331A (en) * 2020-11-18 2021-02-05 江西信达航科新材料科技有限公司 High-temperature-resistant antioxidant composite coating and preparation process thereof

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US6478994B1 (en) * 2000-03-30 2002-11-12 Trustees Of The University Of Pennsylvania Method for making boron carbide containing ceramics
US8320727B1 (en) * 2008-01-11 2012-11-27 Hrl Laboratories, Llc Composite structures with ordered three-dimensional (3D) continuous interpenetrating phases
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US9388042B2 (en) * 2011-02-25 2016-07-12 Rutgers, The State University Of New Jersey Scalable multiple-inverse diffusion flame burner for synthesis and processing of carbon-based and other nanostructured materials and films and fuels
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