CN107585749B - Boron nitride nanosheet powder, green macro-preparation method and application thereof - Google Patents
Boron nitride nanosheet powder, green macro-preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses boron nitride nanosheet powder, a green macro-preparation method and application thereof. The green macro preparation method comprises the following steps: mixing a boron source and a carrier to serve as a precursor, heating to 700-1100 ℃ in an ammonia atmosphere, preserving heat for 60-180 min, cooling to room temperature in a protective atmosphere to obtain a crude product, and performing post-treatment on the crude product to obtain a large amount of pure boron nitride nanosheet powder, wherein the boron source comprises boron oxide, and the carrier comprises sodium chloride and/or potassium chloride. The preparation method disclosed by the invention is simple in preparation process, green and pollution-free, cheap and easily available in raw materials, safe and non-toxic, the conversion rate of a boron source can reach 89%, and the obtained boron nitride nanosheet powder is a hexagonal boron nitride nanosheet, and the purity of the hexagonal boron nitride nanosheet is more than 99%. The invention can realize gram-grade batch green production of high-purity boron nitride nanosheet powder.
Description
Technical Field
The invention particularly relates to a method for green macro-preparation of boron nitride nanosheet powder, and belongs to the technical field of inorganic nano materials.
Background
Boron nitride has a structure similar to that of graphite and belongs to a hexagonal system, in-plane B atoms and N atoms are bonded by covalent bonds, and in-plane atoms are bonded by van der waals forces. The boron nitride family contains a plurality of members such as boron nitride nanosheets, boron nitride nanotubes, boron nitride nanoribbons, boron nitride aerogel, boron nitride quantum dots and the like, wherein the hexagonal boron nitride nanosheets are important wide-bandgap semiconductor materials, the forbidden bandwidth of the hexagonal boron nitride nanosheets reaches 5-6 eV, the hexagonal boron nitride nanosheets have excellent physicochemical properties such as excellent thermal conductivity, chemical stability, excellent insulativity, hydrophobicity, large specific surface area, good biocompatibility, good high temperature resistance and oxidation resistance and the like, and can be widely applied to high-tech fields such as machinery, electronics, aerospace, biomedicine and the like. Obviously, these excellent properties of boron nitride nanosheets not only provide fundamental research, but also provide great potential for the development of advanced materials and wider practical applications. Therefore, the preparation of the boron nitride nanosheet becomes one of the important research directions in the field of boron nitride nanomaterials nowadays.
According to the report, Pacil firstly prepares the boron nitride nanosheet by a mechanical stripping method, and the specific method is that hexagonal boron nitride powder with the particle size of 10 microns is adhered to a silicon dioxide substrate with the thickness of 300nm by using an adhesive tape, then the boron nitride is forcedly separated into small fragments, and finally the two-dimensional boron nitride nanosheet with the thickness of only a few atomic layers is obtained. Then, some researchers have developed moreMethods, techniques for preparing boron nitride nanoplates, such as ball milling, ultrasonic assisted lift-off, chemical vapor deposition, wet chemistry, and the like. Compared with a mechanical stripping method, the ball milling method can obtain a larger amount of boron nitride nanosheets. For example, Li et al reported a mild wet ball milling method that resulted in boron nitride nanoplatelets of a few atomic layer thicknesses with slightly reduced size and good crystallinity of the nanoplatelets. For another example, Lin and the like prove that under the ultrasonic-assisted action, water can effectively strip boron nitride, and a water-soluble boron nitride nanosheet can be obtained on the premise of not adding any surfactant and functional modification. The preparation of boron nitride nanosheets by chemical vapor deposition dates back to 1968, and the use of diborane (B) by Rand et al2H6) And ammonia (NH)3) As a precursor, the precursor is deposited on different substrates within the range of 600-1080 ℃. For wet chemistry, Rao et al use boric acid (H)3BO3) And urea (CO (NH)2)2) In N2Heating to 900 ℃ under protection to obtain the boron nitride nanosheet with the thickness of several atomic layers.
Although a plurality of methods for preparing the boron nitride nanosheets exist, the method is difficult to realize the consideration of yield, cost, crystallinity, environmental protection and the like, and the application of the boron nitride nanosheets is limited to a great extent.
Therefore, the method for preparing boron nitride nanosheet powder in a green and macroscopic manner has very urgent practical needs.
Disclosure of Invention
The invention mainly aims to provide boron nitride nanosheet powder, a green macro-preparation method and application thereof, so as to overcome the defects in the prior art.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a method for green macro-preparation of boron nitride nanosheet powder, which comprises the following steps:
providing a precursor formed by mixing a boron source and a carrier, wherein the boron source comprises boron oxide and the carrier comprises sodium chloride and/or potassium chloride;
heating the precursor to 700-1100 ℃ in an ammonia atmosphere, preserving the heat for 60-180 min in the atmosphere, then cooling to room temperature in a protective atmosphere to obtain a crude product, and performing post-treatment on the crude product to obtain macroscopic quantity of pure boron nitride nanosheet powder.
In a preferred embodiment, the boron source is boron oxide.
In a preferred embodiment, the carrier is sodium chloride and/or potassium chloride.
The embodiment of the invention also provides the boron nitride nanosheet powder prepared by the method.
The embodiment of the invention also provides application of the boron nitride nanosheet powder.
Compared with the prior art, the invention has the advantages that: the process for preparing boron nitride nanosheet powder in a green and macroscopic manner is simple and easy to operate, the reaction can be completed by only one step to obtain a powdery crude product, the adopted raw materials are boron oxide and a carrier (sodium chloride and/or potassium chloride), the raw materials are low in price and easy to purchase, green and pollution-free, water-soluble and the like, the conversion rate of the boron oxide in the raw materials is more than 89%, green preparation of gram-grade boron nitride nanosheet powder can be easily realized through single batch reaction, in addition, the post-treatment operation of the obtained crude product is simple and green and environment-friendly, and the purity of the obtained target product after treatment is up to 99%.
Drawings
Fig. 1 is a photograph of a crude product of boron nitride nanosheet obtained in example 1 without being washed with water.
FIG. 2 is a photograph of a boron nitride nanosheet after post-treatment of the crude product obtained in example 1.
Fig. 3 is an XRD pattern of the water-washed boron nitride nanosheet obtained in example 1.
FIGS. 4 a-4 b are SEM and TEM images of the large-lamellar boron nitride nanosheets obtained in example 1, respectively.
FIGS. 5 a-5 b are SEM and TEM images of the platelet-shaped boron nitride nanosheets obtained in example 1, respectively.
Fig. 6 is an XRD pattern of the boron nitride nanosheet obtained in example 2.
FIG. 7 is a photograph of a boron nitride nanosheet taken after post-treatment of the crude product of example 3.
Fig. 8 is a photograph of a crude product of boron nitride nanosheet obtained in example 4 without being washed with water.
Fig. 9 is an XRD pattern of the boron nitride nanosheet obtained in example 4 after washing with water.
Fig. 10 is an SEM image of the boron nitride nanosheets obtained in example 5.
Detailed Description
In view of the defects in the prior art, the inventor of the present invention has made extensive research and long-term exploration, and proposes the technical scheme of the present invention, which mainly relates to a method for green macro preparation of boron nitride nanosheet powder, as will be described in detail below.
The method for green macro-preparation of the boron nitride nanosheet powder provided by the embodiment of the invention comprises the following steps:
providing a precursor formed by mixing a boron source and a carrier, wherein the boron source comprises boron oxide and the carrier comprises sodium chloride and/or potassium chloride;
heating the precursor to 700-1100 ℃ in an ammonia atmosphere, carrying out heat preservation reaction in the ammonia atmosphere, then cooling to room temperature in a protective atmosphere to obtain a crude product, and carrying out post-treatment on the crude product to obtain a macroscopic quantity of pure boron nitride nanosheet powder.
Preferably, the mass ratio of the boron source to the carrier is 1: 3.
Preferably, the boron source is boron oxide.
Preferably, the carrier is sodium chloride and/or potassium chloride.
In some preferred embodiments, the post-treatment comprises: and soaking the crude product in deionized water for 30-60 min, separating out solid matters, and drying at 40-60 ℃ for 60-120 min to obtain macroscopic quantity of pure boron nitride nanosheet powder.
The solid may be separated by filtration, centrifugation, or the like, but is not limited thereto.
Further, the protective atmosphere may be selected from inert atmospheres, such as argon atmospheres.
Further, the pure boron nitride nanosheet powder is a hexagonal boron nitride nanosheet with the purity of more than 99%.
In some embodiments, the green color preparation method comprises: the mixture of boron oxide and sodium chloride is used as a precursor, and the obtained pure boron nitride nanosheet powder comprises hexagonal boron nitride nanosheets which are arranged compactly and have the size of 90-120 nm and hexagonal boron nitride nanosheets which have the content of less than 5wt% and have the size of 20-50 mu m.
In some preferred embodiments, the green preparation method comprises: the mixture of boron oxide and potassium chloride is used as a precursor, and the obtained pure boron nitride nanosheet powder is a uniform hexagonal boron nitride nanosheet with the size of 90-120 nm.
That is, in some embodiments, if a mixture of boron oxide and sodium chloride is used as a precursor, the hexagonal boron nitride nanoplates comprise two morphologies: one is a densely arranged small sheet layer and one is a thin large sheet layer; if the mixture of boron oxide and potassium chloride is used as a precursor, the hexagonal boron nitride nanosheets are uniform small nanosheets.
In some specific embodiments of the invention, a method for green macro-preparation of boron nitride nanosheet powder comprises the following steps:
(1) and fully mixing a boron source and a carrier to be used as a precursor, heating to 700-1100 ℃ in an ammonia atmosphere, preserving heat for 60-180 min, and then cooling to room temperature in an argon protective atmosphere to obtain a crude product of powder.
(2) And (2) washing, filtering and drying the crude product obtained in the step (1) to obtain the boron nitride nanosheet powder with the purity of more than 99%.
By means of the scheme, the proportion and the dosage of the boron oxide and the carrier are regulated, and the yield of the pure boron nitride nanosheet powder obtained in a single batch can reach gram level or above.
In a specific embodiment, the preparation method involves the following chemical reactions:
B2O3+2NH3→2BN+3H2O。
the reaction temperature in step (1) is preferably: the product has good crystallinity at 1000-1100 ℃.
The water washing and filtering in the step (2) are preferably as follows: and 2-3 times of deionized water cleaning is performed in the filtering process, so that the purity of the boron nitride nanosheet powder can be improved.
The drying in step (2) is preferably: drying at 60 deg.C.
The embodiment of the invention also provides the boron nitride nanosheet powder prepared by the method.
The hexagonal boron nitride nanosheet obtained by the method can be applied to the fields of electronic packaging insulating and heat dissipating materials, heat conducting oil fillers, heat conducting and insulating fillers of composite materials, lubricating materials, drug loads, catalyst carriers and the like.
The technical solution of the present invention is described in more detail below with reference to the accompanying drawings and some exemplary embodiments:
example 1 0.3g B2O3Thoroughly mixed with 0.5g NaCl, placed in an open alumina crucible, then placed in the quartz tube of a tube furnace, and NH was introduced into the tube furnace at 200 standard milliliters per minute (sccm)3The temperature was raised to 1100 ℃. After reacting for 120min at the constant temperature of 1100 ℃, closing NH3Ar of 200sccm is introduced, and the temperature is reduced to room temperature in an Ar atmosphere, and the obtained crude product is taken out. Soaking and cleaning the obtained crude product with deionized water for 30-60 min, carrying out vacuum filtration, and drying in an oven at 60 ℃ for 60-120 min to obtain the boron nitride nanosheet powder with the purity of more than 99%. Fig. 1 is a photograph of a crude product of boron nitride nanosheet obtained in this example without being washed with water. Fig. 2 is a photograph of a boron nitride nanosheet in the present example after-treatment of the crude product. Fig. 3 is an XRD pattern of the boron nitride nanosheet obtained in this example after washing with water, and it can be confirmed that the product is hexagonal boron nitride. Fig. 4a to 4b are SEM and TEM images of the boron nitride nanosheets obtained in this example, respectively, and large-size layers of the boron nitride nanosheets can be observed. Fig. 5 a-5 b are SEM and TEM images of BNNS obtained in this example, and a platelet layer of boron nitride nanosheet can be observed.
Example 2 0.3g B was taken2O3And 0.5g NaCl, placed in an open alumina crucible, then placed in the quartz tube of a tube furnace, and 200 standard milliliters per minute (sccm) of NH was introduced3The temperature was raised to 700 ℃. After the reaction is carried out for 120min at the constant temperature of 700 ℃, NH is closed3Ar of 200sccm is introduced, and the temperature is reduced to room temperature in an Ar atmosphere, and the obtained crude product is taken out. Soaking and cleaning the obtained crude product with deionized water for 30-60 min, carrying out vacuum filtration, and drying in an oven at 60 ℃ for 60-120 min to obtain the boron nitride nanosheet powder with the purity of more than 99%. Fig. 6 is an XRD pattern of the boron nitride nanosheet obtained in this example.
Example 3 example 1.2g B2O3And 8.4g NaCl by gentle grinding in a mortar, placed in an open alumina crucible, and then placed in a quartz tube of a tube furnace, and 200 standard milliliters per minute (sccm) of NH was introduced3The temperature was raised to 1100 ℃. NH is closed after the reaction is carried out for 180min at the constant temperature of 1100 DEG C3Ar of 200sccm is introduced, and the temperature is reduced to room temperature in an Ar atmosphere, and the obtained crude product is taken out. Soaking and cleaning the obtained crude product with deionized water for 30-60 min, carrying out vacuum filtration, and drying in an oven at 60 ℃ for 60-120 min to obtain the boron nitride nanosheet powder with the purity of more than 99%. In this example, the boron oxide conversion rate was 89%. Fig. 7 is a photograph of a boron nitride nanosheet in the present example after-treatment of the crude product.
Example 4 0.3g B2O3And 0.5g NaCl by slight grinding with a mortar to mix thoroughly, placing in an open alumina crucible, placing in a quartz tube of a tube furnace, introducing 200 standard milliliters per minute (sccm) of Ar, heating to 700 deg.C, shutting off the argon, introducing 200sccm of NH3And NH is closed after the reaction is carried out for 120min at the constant temperature of 700 DEG C3Ar of 200sccm is introduced, and the temperature is reduced to room temperature in an Ar atmosphere, and the obtained crude product is taken out. Soaking and cleaning the obtained crude product with deionized water for 30-60 min, carrying out vacuum filtration, and drying in an oven at 60 ℃ for 60-120 min to obtain the boron nitride nanosheet powder with the purity of more than 99%. Fig. 8 is a photograph of a real object of the crude product of boron nitride nanosheet obtained in this example without being washed with water. Fig. 9 is an XRD pattern of the boron nitride nanosheet obtained in this example after washing with water.
Example 5 example 0.3g B2O3Mixing with 0.5g KCl, placing in an open alumina crucible, placing in a quartz tube of a tube furnace, and introducing 200 standard milliliters per minute (sccm) of NH3The temperature was raised to 1100 ℃. After reacting for 120min at the constant temperature of 1100 ℃, closing NH3Ar of 200sccm is introduced, and the temperature is reduced to room temperature in an Ar atmosphere, and the obtained crude product is taken out. Soaking and cleaning the obtained crude product with deionized water for 30-60 min, carrying out vacuum filtration, and drying in an oven at 60 ℃ for 60-120 min to obtain the boron nitride nanosheet powder with the purity of more than 99%. Fig. 10 is an SEM image of the boron nitride nanosheets obtained in this example.
The above examples of the present invention are provided for illustrative clarity, and are not intended to limit the embodiments of the present invention, and all embodiments are not necessarily or exclusively intended to be exhaustive. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. However, any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (5)
1. A method for preparing boron nitride nanosheet powder in a green and macroscopic manner is characterized by comprising the following steps:
providing a precursor which is mainly formed by fully mixing a boron source and a carrier, wherein the boron source comprises boron oxide, the carrier is selected from sodium chloride and/or potassium chloride, and the mass ratio of the boron source to the carrier is 3: 1-1: 7;
heating the precursor to 700-1100 ℃ in an ammonia atmosphere, preserving the heat for 60-180 min in the ammonia atmosphere, then cooling to room temperature in a protective atmosphere to obtain a crude product, and performing post-treatment on the crude product to obtain a macroscopic quantity of pure boron nitride nanosheet powder, wherein the pure boron nitride nanosheet powder is a hexagonal boron nitride nanosheet with the purity of more than 99%;
the method comprises the following steps of (1) adopting a mixture of boron oxide and sodium chloride as a precursor, wherein the obtained pure boron nitride nanosheet powder comprises hexagonal boron nitride nanosheets which are densely arranged and have the size of 90-120 nm and hexagonal boron nitride nanosheets which have the content of below 5wt% and have the size of 20-50 mu m;
the mixture of boron oxide and potassium chloride is used as a precursor, and the obtained pure boron nitride nanosheet powder is a hexagonal boron nitride nanosheet with the size of 90-120 nm.
2. The green macro-preparation method of boron nitride nanosheet powder according to claim 1, wherein the post-treatment comprises: and soaking the crude product in deionized water for 30-60 min, separating out solid matters, and drying at 40-60 ℃ for 60-120 min to obtain macroscopic quantity of pure boron nitride nanosheet powder.
3. The green macro-preparation method of boron nitride nanosheet powder according to claim 1, characterized in that: the protective atmosphere is selected from inert atmospheres.
4. A boron nitride nanosheet powder prepared by the method of any one of claims 1-3.
5. Use of the boron nitride nanosheet powder of claim 4 in the preparation of an electronic packaging insulating heat dissipating material, a heat conducting oil filler, a heat conducting insulating filler of a composite material, a lubricating material, a drug loading material or a catalyst carrier.
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| CN108483414B (en) * | 2018-04-16 | 2019-12-10 | 武汉科技大学 | Low-temperature synthesis diamond boron nitride powder based on molten salt growth method and preparation method thereof |
| CN108439356A (en) * | 2018-05-16 | 2018-08-24 | 武汉科技大学 | A kind of ultrathin boron nitride nanosheet and preparation method thereof |
| CN110357049B (en) * | 2019-07-25 | 2022-06-10 | 中国科学院兰州化学物理研究所 | Method for preparing boron nitride quantum dots by ball milling method |
| CN111099596B (en) * | 2019-12-30 | 2022-09-27 | 东北石油大学 | Simple method for coating high-hydrophobicity boron nitride nanosheet thin layer on surface of silicon dioxide aerogel particle |
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