CN112661123B - Preparation method of double-layer strip-shaped boron nitride hierarchical structure and product - Google Patents
Preparation method of double-layer strip-shaped boron nitride hierarchical structure and product Download PDFInfo
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Abstract
The invention relates to a preparation method of a double-layer strip-shaped boron nitride hierarchical structure and a product, wherein the preparation method mainly comprises the steps of putting magnesium borate whisker into a tubular furnace, introducing reaction gas, heating to 950-. The method has the advantages of wide sources of raw materials, simple and convenient synthesis process flow, low energy consumption, high purity of the purified target product up to 99 percent, and contribution to realizing the batch production of the novel boron nitride strip material.
Description
Technical Field
The invention relates to a preparation method of a double-layer banded BN hierarchical structure and a product thereof.
Background
In recent years, the unique mechanical, thermal and electrical properties of carbon-based nanomaterials attract the attention of many researchers, especially carbon nanotubes and graphene. The main difference between boron nitride nanomaterials and the corresponding carbon nanomaterials is the nature of the bonds between the atoms. The C-C bond in the carbon nano material has pure covalent bond characteristic, and sp 2 Limitation of e to N atoms present in hybridized B-N bonds - And in the pair, the B-N bond presents partial ion characteristics, and the mechanical, optical and electrical properties of the boron nitride nano material are greatly influenced. Therefore, the BN-based material can be used as a heat conduction material due to high heat conductivity, can be applied to biological tissue engineering due to piezoelectric property and good biocompatibility, can be applied to the field of photocatalysis due to large specific surface area, and has great application prospects in the fields of hydrogen storage, lubrication, microwave transparent materials and the like.
The boron nitride material has different forms and is diversified, such as a nano tube, a nano rod, a nano sheet, a nano belt, a micro tube and the like. Different boron nitride hierarchical structures may exist on the primary structure of the tube, sheet, etc. due to the special treatment mode. The Boron Nitride Nanobelts (BNNRs) are representative of the band-shaped boron nitride material. At present, BNNRs are mainly prepared by dissociating Boron Nitride Nanotubes (BNNTs), and the synthesis and corresponding application research are few, the synthesis method mainly comprises a gas etching method and an in-situ melting method, wherein the former BNNTs are subjected to post-treatment and are cracked into BNNRs, and the latter BNNRs are in-situ melted during the BNNTs synthesis process to generate BNNRs, but the two methods have no possibility of batch synthesis for a while. In the synthesis of a BN hierarchical structure, a large number of BN nanosheet BN nanowires are loaded, a large number of bird nest-shaped BN hollow spheres of BN nanosheets are distributed on the surface, and BN nanorods which are stacked with the BN nanosheets along the axial direction are explored and synthesized, but the commonly synthesized BN nanorods are low in purity and long in process period.
In the current research, the band-shaped BN material has no possibility of industrial application. The method has the advantages of simple synthesis and high purity, the current situation of the novel strip-shaped material which is gram-grade in single synthesis amount and has industrial application capability is expected to be changed, and the strip-shaped hierarchical structure material loaded with the nanosheets is not reported in documents.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a method for preparing a double-layer band-shaped BN hierarchical structure and a product thereof, aiming at the above-mentioned shortcomings of the prior art. The raw materials are easy to obtain, the synthesis method is favorable for large-scale industrial preparation, and the special BN nanosheet loaded on the surface of the double-layer band-shaped BN can be prepared and has a unique double-layer band-shaped BN structure.
The technical scheme adopted by the invention for solving the problems is as follows:
a double-layer strip-shaped boron nitride hierarchical structure is characterized in that a boron nitride material is in a double-layer strip shape, the bandwidth range is 0.3-2 mu m, the average bandwidth is 0.6-0.8 mu m, the strip length is 5-50 mu m, and the thickness of the double-layer wall is 10-50 nm; the surface of the strip structure is loaded with boron nitride nanosheets with secondary structures, the average thickness of a single nanosheet is 4-6 nm, and the average size of the single nanosheet is 40-60 nm.
The preparation method of the double-layer strip-shaped boron nitride hierarchical structure mainly comprises the following steps:
1) placing the magnesium borate whisker in a tube furnace, heating to 950-1150 ℃ in a nitrogen-containing atmosphere, preserving heat for 1-4 h, and performing acid washing, purification and suction filtration to obtain an initial product;
2) and drying the primary product at the high temperature of 100-150 ℃ for 10-60min to obtain the double-layer band-shaped BN hierarchical structure.
According to the scheme, the magnesium borate whisker is contained on a nickel sheet substrate of an alumina ark.
According to the scheme, the magnesium borate precursor is whisker-shaped, the diameter of the precursor is 0.3-2 mu m, and the length of the precursor is 5-50 mu m.
According to the scheme, the nitrogen-containing atmosphere is N 2 Atmosphere, NH 3 Atmosphere, N 2 And H 2 The flow rate of the nitrogen-containing atmosphere is preferably 50ml/min to 200ml/min, and the optimum flow rate of the atmosphere is 100 ml/min.
According to the scheme, in the step (1), the optimal heat preservation time is 3 hours, and the heat preservation temperature is 1100 ℃.
According to the scheme, the acid washing purification method comprises the following steps: dispersing the solid product obtained by heat preservation in deionized water, adding acid, heating and stirring at 50-80 ℃ for 5-8 h, and then performing suction filtration and washing to complete purification. Wherein, 12mol/L hydrochloric acid and 15mol/L nitric acid can be used as the acid.
The following chemical reactions (taking ammonia as an example of a nitrogen-containing atmosphere) may occur in the process of preparing BN by the nitridation reaction of the commercial magnesium borate precursor in the invention:
Mg 2 B 2 O 5 +2NH 3 →2BN+3H 2 O+2Mg
decomposing ammonia gas to N at about 540 DEG C 2 And H 2 . In the reducing atmosphere, Mg gradually increases with temperature 2 B 2 O 5 The surface layer of the whisker is etched and decomposed to be in a local molten state, and active N atoms and active H atoms are in Mg 2 B 2 O 5 Diffusion reaction on the surface of whisker to form BN, H 2 O and MgO. And with further time, the whiskers are all subjected to reduction nitridation to form a BN hollow structure. Simultaneously, a part of gas phase activity B and active N atoms decomposed by the crystal whisker are deposited at active sites on the surface of BN coated on the surface of the crystal whisker at the later stage, and nucleation and growth are formedA flaky BN nanosheet. And in the later stage, the sample after acid washing and purification is in the drying process, the high-temperature environment reached by the air blowing drying box is utilized, water and absolute ethyl alcohol existing in the initial product BN hollow structure are enabled to be rapidly volatilized in a limited space, so that a negative pressure environment is formed in the BN hollow structure, the outside maintains a normal pressure state, the hollow structure is caused to collapse, and a double-layer strip-shaped BN structure is finally formed.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention takes the commercial magnesium borate crystal whisker which is simple and easy to obtain as a boron source, uses the nickel sheet substrate to carry out nitridation reaction in a tubular furnace, and the XRD analysis proves that the product prepared after post-treatment has no impurity phase, the purity reaches 99 percent, and the conversion rate of boron element reaches more than 90 percent, thereby being beneficial to large-scale industrialized preparation.
2. The invention has simple synthesis process and simple equipment, can be prepared by using a common single-temperature-zone tubular furnace in the nitridation process, has low requirement on temperature control range, high repetition rate and good process stability, and is beneficial to batch production.
3. The high-temperature blast drying post-treatment process plays a key role in forming the double-layer strip-shaped BN structure, and the BN hollow structure can collapse into the unique double-layer strip-shaped BN structure by utilizing a special negative pressure collapse principle that ethanol and water in the micro-nano tube are quickly evaporated at high temperature.
4. The special BN nanosheets are loaded on the surface of the double-layer banded BN prepared by the method, and the structure has considerable application prospects in the fields of reinforcing and toughening of composite materials, reinforcing of heat conductivity of polymers and photocatalysis.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) spectrum of BN obtained in example 1. Wherein, (a), (b), (c) and (d) are the double-layer band-shaped BN hierarchical structure obtained in the step (3); (e) and (f) is a primary product BN hollow tube obtained in the step (1).
Fig. 2 is a surface-scan energy spectrum (EDS) of the double-layer band-like BN hierarchical structure powder obtained in example 1.
Fig. 3 is a Transmission Electron Microscope (TEM) photograph of the double-layered band-like BN hierarchical structure powder obtained in example 1.
Fig. 4 is a surface-scan energy spectrum (EDS) of a single BN band of the double-layer band-shaped BN hierarchical structure powder obtained in example 1.
Fig. 5 is an X-ray diffraction (XRD) pattern of the obtained double-layer band-shaped BN hierarchical structure powder of example 1.
Fig. 6 is an infrared (FTIR) spectrum of the double-layered band-shaped BN hierarchical structure powder obtained in example 1.
Fig. 7 is a Raman (Raman) spectrum of the double-layer band-shaped BN hierarchical structure powder obtained in example 1.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
In the following examples, the morphology of the resulting product was observed with a FEI Quanta FEG model 250 scanning electron microscope (FSEM); researching the internal microstructure of the sample by using a JEM2100-F type Transmission Electron Microscope (TEM), ultrasonically dispersing the product in absolute ethyl alcohol, and dropwise adding the product onto a copper net; x-ray diffraction analysis (XRD) Using an X-ray powder diffractometer model Rigaku D/MAX-LLIA
2 theta is 10-80 degrees; infrared spectroscopy (FTIR) test using Thermo Nexus470 fourier transform infrared spectrometer (thermoelectric high force corporation, usa); raman spectroscopy (Raman) testing was performed using a Thermo Fisher DXR model laser confocal Raman spectrometer (Raman).
Example 1
A preparation method of a double-layer band-shaped BN hierarchical structure comprises the following steps:
(1) uniformly scattering 5g of commercial magnesium borate whiskers on a nickel sheet substrate of an alumina ark, putting the aluminum borate whiskers into a tubular furnace, vacuumizing, introducing ammonia gas, keeping the temperature at 1050 ℃ for 4 hours, cooling to 200 ℃ along with the furnace, closing a vent valve, and naturally cooling to room temperature to obtain a primary product;
(2) dispersing the primary product in 50ml of distilled water, adding 90ml of 12mol/L hydrochloric acid, 6ml of HNO3 and 40ml of absolute ethyl alcohol, heating and stirring at 50 ℃ for 5 hours, washing with deionized water, centrifuging three times, washing with ethanol twice, and finally blowing and drying for 10min at-1 KPa and 150 ℃ to obtain 1.54g of a film consisting of double-layer strip boron nitride, wherein the conversion rate of boron element is 93.46%.
(3) Dispersing the double-layer band-shaped boron nitride film in 50ml of absolute ethyl alcohol, centrifuging at the speed of 800r/min, separating supernatant, and re-drying the lower-layer precipitate under the conditions of normal pressure and the temperature of 40 ℃ to obtain double-layer band-shaped BN hierarchical structure powder.
As shown in fig. 1, the SEM spectrum of the BN sample prepared in this example. As shown in FIG. 1 (a), the structure is similar to a sea-belt shape, the band width ranges from 0.4 to 2 μm, the band length ranges from 5 to 50 μm, and the morphology is uniform. As can be seen from the white circles in fig. 1 (b), the structure surface is loaded with a certain amount of BN nanosheets, and the size of individual flakes is about 5 nm. As can be seen from (c) of FIG. 1, the structure exhibits a double-layer structure, and the thickness of the double-layer strip is 10 to 50 nm. As shown in fig. 2, EDS of the BN sample prepared in this example. As shown in fig. 2 (b) and (c), the sample is composed of B, N elements and is distributed uniformly. In FIG. 1, (e) and (f) are schematic hollow tube diagrams of primary BN, it can be seen that the morphology changes greatly after high-temperature drying, and double-layer band-shaped BN in (a), (b), (c) and (d) is formed.
As shown in fig. 3, HRTEM of the BN sample prepared in this example was taken. As can be seen from the graph (a), the sample morphology is flat, and a small amount of BN sheet is loaded on the surface. From the graph (b), clear lattice fringes can be observed with a lattice spacing of about 0.34nm, which is consistent with the lattice constant of the (002) crystal plane of h-BN, indicating that the h-BN material is.
As shown in fig. 4, the EDS of the sample prepared in this example, a single double-layer band-like BN hierarchical structure. As can be seen from FIGS. (b) and (c), the sample was composed of B, N and was uniformly distributed.
As shown in fig. 5, the XRD pattern of the BN sample prepared in this example. The spectrogram has 5 obvious main diffraction peaks which are respectively positioned at the positions of 2 theta, 26.71 degrees, 42.61 degrees, 45.56 degrees, 55.06 degrees and 75.95 degrees and correspond to (002), (101), (004), (110) and (112) crystal faces (JCPDF No.34-0421) of the h-BN crystal, so that the product has no impurity phases and high purity.
As shown in FIG. 6, the FTIR spectrum of the BN sample prepared in this example has 3 distinct characteristic absorption peaks respectively located at 812, 1380 and 3420cm -1 To (3). Of these, 812 and 1380cm -1 The absorption peaks at (B) and (B) respectively correspond to the in-plane stretching vibration of the B-N bond in the h-BN material, and are 3420cm -1 The absorption peak at (A) is usually due to the absorption of water or stretching vibration of O-H bonds in the slight oxidation of the surface.
As shown in FIG. 7, the Raman spectrum of the BN sample prepared in this example was found to be 1361cm -1 In-plane E having a scattering peak of BN 2g Vibration, consistent with literature reports.
The above map analysis results prove that: the prepared sample has a hexagonal boron nitride crystal structure without impurity phases.
Example 2
A preparation method of a BN tape with a double-layer tape-shaped structure comprises the following steps:
(1) uniformly scattering 5g of commercial magnesium borate whiskers on a nickel sheet substrate of an alumina ark, putting the aluminum borate whiskers into a tubular furnace, vacuumizing, introducing ammonia gas, keeping the temperature of 1150 ℃ for 4 hours, cooling the aluminum borate whiskers to 200 ℃ along with the furnace, closing a vent valve, and naturally cooling the aluminum borate whiskers to room temperature to obtain a primary product;
(2) dispersing the primary product in 50ml of distilled water, adding 90ml of 12mol/L hydrochloric acid, 6ml of HNO3 and 40ml of absolute ethyl alcohol, heating and stirring at 50 ℃ for 5h, washing with deionized water, centrifuging three times, washing with ethanol twice, and finally blowing and drying for 30min at-0.95 KPa and 120 ℃ to obtain 1.56g of a film consisting of double-layer strip boron nitride, wherein the conversion rate of boron element is 94.27%.
(3) Dispersing the double-layer band-shaped boron nitride film in 50ml of absolute ethyl alcohol, centrifuging at the speed of 800r/min, separating supernatant, and re-drying the lower-layer precipitate under the conditions of normal pressure and the temperature of 40 ℃ to obtain double-layer band-shaped BN hierarchical structure powder.
Example 3
A preparation method of a double-layer band-shaped BN hierarchical structure comprises the following steps:
(1) uniformly scattering 10g of commercial magnesium borate whiskers on a nickel sheet substrate of an alumina ark, putting the aluminum borate whiskers into a tubular furnace, vacuumizing, introducing ammonia gas, keeping the temperature at 1100 ℃ for 3 hours, cooling the aluminum borate whiskers to 200 ℃ along with the furnace, closing a vent valve, and naturally cooling the aluminum borate whiskers to room temperature to obtain a primary product;
(2) dispersing the primary product in 80ml distilled water, 12mol/L hydrochloric acid 120ml, 8ml HNO3, 60ml absolute ethyl alcohol, 8ml HNO 3 Heating and stirring for 5h at 50 ℃, washing with deionized water and centrifuging for three times, washing with ethanol for two times, and finally blowing and drying for 30min at-1 KPa and 150 ℃ to obtain 3.15g of double-layer strip-shaped boron nitride film with the boron element conversion rate of 95.33%.
(3) Dispersing the double-layer strip-shaped boron nitride film in 50ml of absolute ethyl alcohol, centrifuging at the speed of 800r/min, separating supernatant, and drying the lower-layer precipitate again under the conditions of normal pressure and the temperature of 40 ℃ to obtain double-layer strip-shaped BN hierarchical structure powder.
Example 4
A preparation method of a double-layer band-shaped BN hierarchical structure comprises the following steps:
(1) uniformly scattering 10g of commercial magnesium borate whiskers on a nickel sheet substrate of an alumina ark, putting the aluminum borate whiskers into a tubular furnace, vacuumizing, introducing ammonia gas, keeping the temperature at 950 ℃ for 2 hours, cooling to 200 ℃ along with the furnace, closing a vent valve, and naturally cooling to room temperature to obtain a primary product;
(2) dispersing the primary product in 60ml distilled water, 12mol/L hydrochloric acid 120ml, 8ml HNO3, 50ml absolute ethyl alcohol, heating and stirring at 50 ℃ for 5h, washing with deionized water and centrifuging three times, and washing with ethanol two times
And finally, blowing and drying for 20min at-90 KPa and 120 ℃ to obtain 2.99g of film consisting of double-layer strip boron nitride, wherein the conversion rate of boron element is 90.76%.
(3) Dispersing the double-layer strip-shaped boron nitride film in 50ml of absolute ethyl alcohol, centrifuging at the speed of 800r/min, separating supernatant, and drying the lower-layer precipitate again under the conditions of normal pressure and the temperature of 40 ℃ to obtain double-layer strip-shaped BN hierarchical structure powder.
Example 5
A preparation method of a double-layer band-shaped BN hierarchical structure comprises the following steps:
(1) uniformly scattering 10g of commercial magnesium borate whiskers on a nickel sheet substrate of an alumina ark, putting the aluminum borate whiskers into a tubular furnace, vacuumizing, introducing ammonia gas, keeping the temperature at 1000 ℃ for 1h, cooling to 200 ℃ along with the furnace, closing a vent valve, and naturally cooling to room temperature to obtain a primary product;
(2) dispersing the primary product in 60ml of distilled water, adding 120ml of 12mol/L hydrochloric acid, 8ml of HNO3 and 50ml of absolute ethyl alcohol, heating and stirring at 50 ℃ for 5 hours, washing with deionized water, centrifuging three times, washing with ethanol twice, and finally blowing and drying for 60 minutes at-0.95 KPa and 100 ℃ to obtain 3.05g of a film consisting of double-layer strip-shaped boron nitride, wherein the conversion rate of boron element is 92.47%.
(3) The double-layer strip-shaped boron nitride film is dispersed in 50ml of absolute ethyl alcohol, and the powder with the double-layer strip-shaped BN hierarchical structure is obtained at the speed of 800 r/min.
The embodiments described above are only for illustrating the technical idea and features of the present invention, and it should be noted that equivalent changes and modifications made without departing from the inventive idea of the present invention are all covered within the protection scope of the present invention.
Claims (8)
1. A double-layer strip-shaped boron nitride hierarchical structure is characterized in that the structure is in a double-layer strip shape, the bandwidth range is 0.3-2 mu m, the average bandwidth is 0.6-0.8 mu m, the strip length is 5-50 mu m, and the thickness of the double-layer wall is 10-50 nm; the surface of the strip structure is loaded with boron nitride nanosheets with secondary structures, the average thickness of a single nanosheet is 4-6 nm, and the average size of the single nanosheet is 40-60 nm.
2. The method for preparing a double-layer strip-shaped boron nitride hierarchical structure according to claim 1 is characterized by mainly comprising the following steps:
1) putting the magnesium borate whisker into a tubular furnace, heating to 950-1150 ℃ in a nitrogen-containing atmosphere, preserving heat for 1-4 h, and performing acid cleaning, purification and suction filtration to obtain an initial product;
2) and drying the primary product at the high temperature of 100-150 ℃ for 10-60min to obtain the double-layer band-shaped BN hierarchical structure.
3. The method of claim 2, wherein the magnesium borate whiskers are placed on an alumina ark with a nickel plate base.
4. The method for preparing the double-layer strip-shaped boron nitride hierarchical structure according to claim 2, wherein the magnesium borate whisker has a diameter of 0.3-2 μm and a length of 5-50 μm.
5. The method of claim 2, wherein the nitrogen-containing atmosphere is N 2 Atmosphere, NH 3 Atmosphere, N 2 And H 2 One of mixed atmospheres.
6. The method according to claim 5, wherein the flow rate of the nitrogen-containing atmosphere is 50ml/min to 200 ml/min.
7. The method for preparing a double-layer strip-shaped boron nitride hierarchical structure according to claim 2, wherein the heat preservation time in the step (1) is 3 hours, and the heat preservation temperature is 1100 ℃.
8. The method for preparing a double-layer strip-shaped boron nitride hierarchical structure according to claim 2, wherein the acid cleaning purification method comprises the following steps: dispersing the solid product obtained by heat preservation in deionized water, adding acid, heating and stirring at 50-80 ℃ for 5-8 h, and then performing suction filtration and washing to complete purification.
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