CN108423647B - Method for preparing macroscopic quantity hexagonal boron nitride powder by chemical vapor deposition method - Google Patents
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Abstract
The invention discloses a method for preparing macroscopic quantity hexagonal boron nitride powder by a chemical vapor deposition method, which comprises the following steps: heating a precursor to 900-1450 ℃ in a nitrogen-containing reaction atmosphere, preserving heat, and then cooling to room temperature in a protective atmosphere to obtain a crude product, wherein the precursor comprises a uniform mixture of boron oxide and magnesium chloride; and carrying out post-treatment on the crude product, thereby obtaining the hexagonal boron nitride powder. The raw materials adopted by the process are cheap and easy to obtain, the process flow is simple, the crude product can be obtained in one step, the reaction efficiency of the precursor is as high as 95 percent, the crude product can be subjected to simple post-treatment to form a product with the purity of 99 percent, and two hexagonal boron nitride powder products with completely different shapes and functions can be obtained only by changing the reaction temperature range in the process. The process of the invention can easily realize the preparation of hexagonal boron nitride above gram level.
Description
Technical Field
The invention particularly relates to a method for preparing macroscopic quantity hexagonal boron nitride powder by a chemical vapor deposition method, belonging to the technical field of inorganic nano materials.
Background
Boron nitride has four different variant structures: hexagonal Boron Nitride (HBN), Rhombohedral Boron Nitride (RBN), Cubic Boron Nitride (CBN), and Wurtzite Boron Nitride (WBN). The hexagonal boron nitride which is very important is white, is a classic graphene-like layered structure, has excellent high thermal conductivity (the thermal conductivity is ten times of that of quartz), high temperature resistance (the melting point is 3000 ℃), oxidation resistance (oxidation starts in air at the temperature of more than 1200 ℃), electrical insulation, hydrophobicity, lubrication, good chemical stability (acid and alkali resistance), biocompatibility and the like, and is also called white graphite. There are also a number of members in the hexagonal boron nitride subfamily such as: boron nitride films, boron nitride nanosheets, boron nitride nanotubes, porous boron nitride, boron nitride nanoribbons, boron nitride fibers, and the like. The boron nitride film has good application prospect in the fields of graphene electronic devices and deep ultraviolet light emission; the boron nitride nanosheet, the boron nitride nanotube and the boron nitride fiber are very important heat dissipation fillers in the field of heat management of electronic packaging, and play an important role in the fields of lubrication and friction; the porous boron nitride is a very excellent self-cleaning environment-friendly material by virtue of the advantages of porosity and hydrophobicity, and plays an important role in removing dirt in the aspects of oil absorption, organic solvents, dyes and the like.
The existing methods for preparing hexagonal boron nitride are also various, such as a mechanical stripping method and a solution stripping method, and are mainly used for preparing boron nitride nanosheets (Angew. chem. int. Ed.2012,51, 6498-; a chemical bubbling method, which mainly prepares boron nitride nano-sheets (Adv mater.2011,23, 4072-; chemical solvent synthesis method, can prepare high specific surface area boron nitride (nat. Commun.2013.4: 1777); the carbon-based material can be used for preparing boron nitride nanotubes, boron nitride nanosheets (ACS Nano No.2014, 8,9081-9088) and the like through high-temperature replacement reaction; the method can prepare hexagonal boron nitride materials with various shapes and functions, such as boron nitride films, boron nitride Nano sheets, boron nitride nanotubes, porous boron nitride, boron nitride nanobelts, boron nitride fibers and the like, by changing the precursor and the growth conditions (Nano Lett.2012,12, 161-166).
Although the existing preparation methods are rich and various, due to the limitation of experiments, the preparation methods are difficult to realize superiority in the aspects of large yield, high crystallinity, low cost, environment-friendly property and the like, and the industrial development process of boron nitride is severely restricted by high cost and low efficiency. Therefore, the exploration of a simple and efficient preparation technology of the hexagonal boron nitride has very important scientific research value and practical significance.
Disclosure of Invention
The invention mainly aims to provide a method for preparing macroscopic quantity hexagonal boron nitride powder by a chemical vapor deposition method so as to overcome the defects of the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a method for preparing macroscopic quantity hexagonal boron nitride powder by a chemical vapor deposition method, which comprises the following steps:
heating a precursor to 900-1450 ℃ in a nitrogen-containing reaction atmosphere, preserving heat, and then cooling to room temperature in a protective atmosphere to obtain a crude product, wherein the precursor comprises a uniform mixture of boron oxide and magnesium chloride;
and carrying out post-treatment on the crude product to obtain hexagonal boron nitride powder.
In some embodiments, the molar ratio of boron oxide to magnesium chloride is preferably 2: 3.
In some embodiments, the method for preparing the macroscopic amount of hexagonal boron nitride powder by the chemical vapor deposition method comprises the following steps: and carrying out solid-phase mixing on the boron oxide and magnesium chloride to form the precursor, wherein the solid-phase mixing method includes grinding, stirring and the like, and is not limited thereto.
In some preferred embodiments, the method for preparing the macroscopic quantity hexagonal boron nitride powder by the chemical vapor deposition method comprises the following steps: and heating the precursor to 900-1450 ℃ in a nitrogen-containing reaction atmosphere, preserving the heat for 60-180 min, and then cooling to room temperature in a protective atmosphere to obtain a crude product.
Further, the nitrogen-containing reaction atmosphere includes, but is not limited to, an ammonia gas atmosphere, and the like.
Further, the protective atmosphere includes nitrogen and/or argon atmosphere, such as nitrogen atmosphere, argon atmosphere, nitrogen and argon mixed atmosphere, and the like, and is not limited thereto.
In some embodiments, the post-treatment comprises: and (3) acid-washing and drying the crude product to obtain macroscopic fluffy hexagonal boron nitride powder.
In some preferred embodiments, the post-treatment comprises: soaking the crude product in an acid solution for 8-12 h, then washing with deionized water, and then drying at 60-80 ℃ for 6-12 h to obtain macroscopic fluffy hexagonal boron nitride powder; the acid solution is preferably a low-concentration acid solution.
Furthermore, the purity of the hexagonal boron nitride powder is more than 99%.
Furthermore, the hexagonal boron nitride powder comprises macroscopically fluffy porous boron nitride powder and/or macroscopically fluffy high-crystallinity boron nitride nanosheets, wherein the specific surface area of the porous boron nitride powder is 140-151 m2/g, and/or an average pore diameter of 5.84 nm.
Further, the method may include: heating the precursor to 1000-1100 ℃ in a nitrogen-containing reaction atmosphere, preserving heat, cooling to room temperature in a protective atmosphere to obtain the crude product, and performing post-treatment on the crude product to obtain the macroscopic fluffy porous boron nitride powder.
Further, the method may include: heating the precursor to 1400-1450 ℃ in a nitrogen-containing reaction atmosphere, preserving heat, cooling to room temperature in a protective atmosphere to obtain the crude product, and performing post-treatment on the crude product to obtain the macroscopic fluffy high-crystallinity boron nitride nanosheet.
Compared with the prior art, the invention has the advantages that:
1. the method for preparing the macroscopic quantity of boron nitride powder by the chemical vapor deposition method provided by the invention adopts boron oxide and metal chloride as raw materials, both are cheap and easily available materials, the process flow is simple, and a crude product can be obtained in one step;
2. according to the method for preparing the macroscopic quantity boron nitride powder by the chemical vapor deposition method, two hexagonal boron nitride powder products with completely different shapes and functions can be obtained by adopting the same precursor and reaction atmosphere and changing the reaction temperature, and the products have potential application values in various fields;
3. according to the method for preparing the macroscopic quantity of boron nitride powder by the chemical vapor deposition method, the reaction efficiency of the precursor is as high as 95%, and the purity of the product obtained by post-treatment is as high as 99%;
4. the method for preparing the macroscopic quantity of boron nitride powder by the chemical vapor deposition method can easily realize the preparation of hexagonal boron nitride above gram level, and has great promotion effect on the industrialization process of the hexagonal boron nitride.
Drawings
FIG. 1 is a photograph of a crude hexagonal boron nitride product of example 1 of the present invention;
FIG. 2 is a photograph of a hexagonal boron nitride powder subjected to post-treatment in example 1 of the present invention;
FIG. 3 is an SEM photograph of hexagonal boron nitride in example 1 of the present invention;
FIG. 4 is a TEM image of hexagonal boron nitride in example 1 of the present invention;
FIG. 5 is an XRD pattern of hexagonal boron nitride in example 1 of the present invention;
fig. 6 is an SEM image of hexagonal boron nitride nanoplates in example 2 of the present invention;
FIG. 7 is a TEM image of hexagonal boron nitride nanosheets in example 2 of the present invention
Fig. 8 is an XRD pattern of hexagonal boron nitride nanosheets in example 2 of the present invention;
fig. 9 is a hydrophobic angle measurement of hexagonal boron nitride nanoplates in example 2 of the present invention.
Detailed Description
In view of the deficiencies in the prior art, the inventors of the present invention have made extensive studies and extensive practices to provide technical solutions of the present invention. The technical solution, its implementation and principles, etc. will be further explained as follows.
One aspect of the embodiments of the present invention provides a method for preparing a macroscopic quantity of hexagonal boron nitride powder by a chemical vapor deposition method, including:
heating a precursor to 900-1450 ℃ in a nitrogen-containing reaction atmosphere, preserving heat, and then cooling to room temperature in a protective atmosphere to obtain a crude product, wherein the precursor comprises a uniform mixture of boron oxide and magnesium chloride;
and carrying out post-treatment on the crude product to obtain hexagonal boron nitride powder.
In a more specific embodiment, boron oxide and magnesium chloride can be uniformly mixed to serve as a precursor and put into a tubular furnace, the mixture is heated to 900-1450 ℃ in an ammonia atmosphere, the temperature is kept at 900-1450 ℃ for 60-180 min, then the temperature is reduced to room temperature in a protective atmosphere to obtain a crude product, and the crude product is subjected to post-treatment to obtain hexagonal boron nitride powder with the purity of more than 99%.
The crude product was a macroscopically fluffy, white crude product.
Further, the post-processing may include: and carrying out acid washing, filtering and drying on the crude product so as to obtain macroscopic fluffy hexagonal boron nitride powder.
By the method, under the optimal synthesis condition, two unique hexagonal boron nitrides can be formed within two specific reaction temperature ranges; the mass of the precursor is adjusted, and the macro preparation of the precursor above gram level can be realized.
In the foregoing embodiment, the preparation method involves the following chemical reaction:
2B2O3(s)+3MgCl2(s)＝2BCl3(g)+Mg3B2O6(s)
BCl3(g)+NH3(g)＝BN(s)+3HCl(g)
Mg3B2O6(s)+2NH3(g)＝2BN(s)+3H2O(g)+3MgO(s)
the general chemical formula is as follows: 2B2O3(s)+3MgCl2(s)+4NH3(g)＝4BN(s)+3H2O(g)+3MgO(s)+6HCl(g)
Side reaction: HCl(g)+NH3(g)＝NH4Cl(g)
Further, the boron oxide and magnesium chloride in the precursor can be mixed according to the weight ratio of 2:3, but of course, other suitable ratios are also possible.
Further, the precursor can be formed by performing solid-phase grinding and mixing on boron oxide and magnesium chloride uniformly.
Further, the precursor can be formed by stirring and mixing the boron oxide and the magnesium chloride in a solid phase.
Further, the protective atmosphere is nitrogen and/or argon atmosphere.
In some embodiments, the post-treatment comprises: soaking the crude product in an acid solution for 8-12 h, washing with deionized water, filtering, and drying at 60-80 ℃ for 6-12 h to obtain macroscopic fluffy hexagonal boron nitride powder with the purity of more than 99%; the acid solution is preferably a low-concentration acid solution.
The low-concentration acid solution may be dilute nitric acid or dilute hydrochloric acid having a concentration of 2.0 mol/L.
Furthermore, at two specific reaction temperatures of 1000 ℃ and 1450 ℃, the following two macroscopic puffs can be mainly obtainedHexagonal boron nitride morphology of (a), i.e.: the specific surface area is 140-151 m2(ii)/g, and/or porous boron nitride powder with an average pore diameter of 5.84nm and high-crystallinity boron nitride nanosheets.
Accordingly, another aspect of the embodiments of the present invention also provides hexagonal boron nitride powder prepared by the above method, namely the above two macroscopically fluffy hexagonal boron nitride morphologies, namely: the specific surface area is 140-151 m2(ii)/g, and/or porous boron nitride powder with an average pore diameter of 5.84nm and high-crystallinity boron nitride nanosheets.
The hexagonal boron nitride powder can play an important role in the fields of decontamination, thermal management of electronic packaging, biological medicine and the like.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed as broadly as the present invention is capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Example 1: b is to be2O3And MgCl2Taking 2g B according to the molar ratio of 2:32O3And 4.1g MgCl2Placing in an alumina crucible, then placing in a quartz tube furnace, and introducing 200sccm NH3Heating to about 1000 ℃, reacting at about 1000 ℃ for 180min at constant temperature, and closing NH3And introducing Ar of 200sccm instead, cooling to room temperature in Ar atmosphere, and taking out to obtain a white macroscopic fluffy crude product. And then soaking the obtained product in 2mol/L dilute hydrochloric acid overnight, filtering and drying to obtain the macroscopic fluffy white porous hexagonal boron nitride powder with the purity of more than 99 percent. FIG. 1 is a photograph of a crude hexagonal boron nitride product prepared in this example. FIG. 2 is a photograph of the hexagonal boron nitride powder after post-treatment according to this example, which can achieve a yield of 95%. Fig. 3 is an SEM image of hexagonal boron nitride obtained in this example, and a clear pore structure can be seen. FIG. 4 shows the present embodimentTEM images of the resulting hexagonal boron nitride. Fig. 5 is an XRD pattern of hexagonal boron nitride obtained in this example, which is confirmed to be hexagonal BN.
Example 2: b is to be2O3And MgCl2Taking 2g B according to the molar ratio of 2:32O3And 4.1g MgCl2Placing in an alumina crucible, placing in an alumina tube furnace, and introducing 200sccm NH3Heating to about 1450 deg.C, reacting at about 1450 deg.C for 180min, and closing NH3And introducing Ar of 300sccm instead, cooling to room temperature in Ar atmosphere, and taking out to obtain a white macroscopic fluffy crude product. And then soaking the obtained product in 2mol/L dilute nitric acid overnight, filtering and drying to obtain macroscopic fluffy white hexagonal boron nitride nanosheet powder with the purity of more than 99%. Fig. 6 is an SEM image of hexagonal boron nitride obtained in the present example, and highly crystalline boron nitride nanosheets can be seen stacked together. FIG. 7 is a TEM image of hexagonal boron nitride obtained in this example. Fig. 8 is an XRD pattern of the hexagonal boron nitride nanosheet obtained in this example without post-treatment, with a significant peak of hexagonal boron nitride, confirming hexagonal structure BN. Fig. 9 is a measurement of the hydrophobic angle of the post-treated hexagonal boron nitride nanosheets, which averaged up to 150 ° in the hydrophobic angle.
In addition, the inventors of the present invention have also conducted experiments using other process conditions described in the present specification with reference to the embodiment of example 1-2, for example, by heating a mixed precursor of boron oxide and magnesium chloride to 900 ℃, 1050 ℃, 1100 ℃, 1300 ℃, 1450 ℃ in the aforementioned nitrogen-containing reaction atmosphere, maintaining the temperature for 180min, 150min, 120min, 100min, 60min, and then cooling the mixed precursor to room temperature in the aforementioned protective atmosphere to obtain a series of crude products, and then post-treating the crude products by the aforementioned post-treatment method to obtain a series of hexagonal fluffy boron nitride powders, which are all in a macroscopic form. Wherein, when the temperature is about 1000 ℃, the obtained porous boron nitride powder has the specific surface area of 140-151 m2/g, and/or an average pore diameter of 5.84 nm. And when the temperature is about 1450 ℃, the obtained boron nitride nanosheet is high in crystallinity.
It should be understood that the above-mentioned embodiments are merely illustrative of the technical concepts and features of the present invention, which are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and therefore, the protection scope of the present invention is not limited thereby. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. A method for preparing macroscopic quantity hexagonal boron nitride powder by a chemical vapor deposition method is characterized by comprising the following steps:
heating the precursor to 900-1450 ℃ in an ammonia atmosphere, preserving heat, and then cooling to room temperature in a protective atmosphere to obtain a crude product, wherein the precursor comprises a uniform mixture of boron oxide and magnesium chloride;
and carrying out post-treatment on the crude product to obtain hexagonal boron nitride powder, wherein the hexagonal boron nitride powder comprises macroscopically fluffy porous boron nitride powder and/or macroscopically fluffy high-crystallinity boron nitride nanosheets.
2. The method for preparing the macroscopic quantity of the hexagonal boron nitride powder by the chemical vapor deposition method according to claim 1, which is characterized in that: the molar ratio of boron oxide to magnesium chloride is 2: 3.
3. The method for preparing the macroscopic quantity of hexagonal boron nitride powder by the chemical vapor deposition method according to claim 1 or 2, which is characterized by comprising the following steps: and carrying out solid-phase mixing on the boron oxide and the magnesium chloride to form the precursor, wherein the adopted solid-phase mixing mode comprises grinding or stirring.
4. The method for preparing the macroscopic quantity of the hexagonal boron nitride powder by the chemical vapor deposition method according to claim 1, which is characterized by comprising the following steps: and heating the precursor to 900-1450 ℃ in an ammonia atmosphere, preserving the temperature for 60-180 min, and then cooling to room temperature in a protective atmosphere to obtain a crude product.
5. The method for preparing the macroscopic quantity of the hexagonal boron nitride powder by the chemical vapor deposition method according to the claim 1 or 4, which is characterized in that: the protective atmosphere comprises a nitrogen and/or argon atmosphere.
6. The method for preparing the macroscopic quantity of the hexagonal boron nitride powder by the chemical vapor deposition method according to claim 1, wherein the post-treatment comprises the following steps: and (3) acid-washing and drying the crude product to obtain macroscopic fluffy hexagonal boron nitride powder.
7. The method for preparing the macroscopic quantity of the hexagonal boron nitride powder by the chemical vapor deposition method according to claim 6, wherein the post-treatment comprises the following steps: and soaking the crude product in an acid solution for 8-12 h, washing with deionized water, and drying at 60-80 ℃ for 6-12 h to obtain macroscopic fluffy hexagonal boron nitride powder.
8. The method for preparing the macroscopic quantity of hexagonal boron nitride powder by the chemical vapor deposition method according to claim 1,6 or 7, which is characterized in that: the purity of the hexagonal boron nitride powder is more than 99%.
9. The method for preparing the macroscopic quantity of the hexagonal boron nitride powder by the chemical vapor deposition method according to claim 8, which is characterized in that: the specific surface area of the porous boron nitride powder is 140-151 m2The average pore diameter of the porous boron nitride powder is 5.84 nm.
10. The method for preparing the macroscopic quantity of the hexagonal boron nitride powder by the chemical vapor deposition method according to claim 9, which is characterized by comprising the following steps:
heating the precursor to 1000-1100 ℃ in an ammonia atmosphere, preserving heat, cooling to room temperature in a protective atmosphere to obtain a crude product, and performing post-treatment on the crude product to obtain macroscopic fluffy porous boron nitride powder;
or heating the precursor to 1400-1450 ℃ in an ammonia atmosphere, preserving heat, cooling to room temperature in a protective atmosphere to obtain the crude product, and performing post-treatment on the crude product to obtain the macroscopic fluffy high-crystallinity boron nitride nanosheet.
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