CN114180540A - Method for adjusting properties of boron nitride aerogel by utilizing atmosphere - Google Patents
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- 239000004964 aerogel Substances 0.000 title claims abstract description 69
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 59
- 239000012298 atmosphere Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000000499 gel Substances 0.000 claims abstract description 24
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 11
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004327 boric acid Substances 0.000 claims abstract description 11
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000009736 wetting Methods 0.000 claims description 5
- 239000012300 argon atmosphere Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000007710 freezing Methods 0.000 claims description 4
- 230000008014 freezing Effects 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims 1
- 229910052796 boron Inorganic materials 0.000 claims 1
- 230000003750 conditioning effect Effects 0.000 claims 1
- 230000001404 mediated effect Effects 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 8
- 238000001179 sorption measurement Methods 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 239000011240 wet gel Substances 0.000 abstract description 5
- 238000012805 post-processing Methods 0.000 abstract description 3
- 230000010354 integration Effects 0.000 abstract description 2
- 239000007783 nanoporous material Substances 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- CTRPRMNBTVRDFH-UHFFFAOYSA-N 2-n-methyl-1,3,5-triazine-2,4,6-triamine Chemical compound CNC1=NC(N)=NC(N)=N1 CTRPRMNBTVRDFH-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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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
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0646—Preparation by pyrolysis of boron and nitrogen containing compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- 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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- Organic Chemistry (AREA)
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Abstract
The invention relates to the field of nano porous materials, in particular to a method for adjusting the properties of boron nitride aerogel by utilizing atmosphere. The supermolecule gel is prepared by taking melamine and boric acid as molecular components, and the supermolecule wet gel can be converted into the boron nitride aerogel under the high-temperature condition after being dried. Changing the atmosphere used during the high temperature conversion process can significantly affect the properties of the resulting aerogel, such as: crystalline state, adsorption behavior, wettability, mechanical properties, etc. The method provided by the invention can realize the integration of synthesis preparation and performance regulation and control, and avoids the intervention of post-processing means for realizing performance regulation. The whole process is simple and convenient, is easy to operate, and is convenient for realizing the mass synthesis of the boron nitride aerogel.
Description
Technical Field
The invention relates to the field of nano porous materials, in particular to a method for adjusting the properties of boron nitride aerogel by utilizing atmosphere.
Background
The aerogel is a porous material with a framework in a nanometer scale, and has wide application prospects in the fields of energy, biology, environment and the like. As one of the new aerogels, boron nitride aerogels have been reported as early as the end of the 20 th century. But the technical limitations make it difficult to synthesize them extensively for downstream applications and research. Recent innovation in preparation means enables the material to reenter the visual field of people, and new possibility is brought to various fields.
A recent series of investigations showed that: the boron nitride aerogel is prepared by taking melamine, methyl melamine and boric acid as components, assembling the components into supramolecular gel by using a supramolecular assembly technology, and treating the supramolecular xerogel at high temperature. The preparation technology comprises two key links: first, the formation of supramolecular gels, i.e. the assembly step; second, the transformation of supramolecular gels, i.e. the high temperature link. The previous research successfully realizes microstructure adjustment by changing various factors in the assembling process, and further influences the apparent performance of the boron nitride aerogel, and specifically comprises two ideas: (1) component strategies, i.e., changing the types and proportions of components (Nanoscale Advances,2020,2, 149-155); (2) solvent strategy, i.e. changing the solvent environment during assembly (iScience,2021,24, 102251).
Previous research has focused primarily on the assembly phase, and the search for the high temperature phase has not been addressed. If a performance regulation strategy aiming at the high-temperature conversion stage can be further developed, the prior art is richer.
Disclosure of Invention
The invention aims to provide a method for adjusting the properties of boron nitride aerogel by utilizing atmosphere, which takes the same supermolecule gel as a precursor, changes the atmosphere type used in a high-temperature transformation link, and influences the properties of the obtained boron nitride aerogel, such as crystallization state, microstructure, wettability, mechanical property and the like.
The technical scheme of the invention is as follows:
a method for adjusting the properties of boron nitride aerogel by utilizing atmosphere, which changes the atmosphere used in a high-temperature conversion stage to influence the properties of the obtained boron nitride aerogel, and comprises the following specific steps:
1) preparation of supramolecular gel: dissolving melamine and boric acid in a molar ratio of 1: 4-1: 8 in deionized water at 70-100 ℃, stirring for 0.1-10 hours to form a solution, pouring the solution into a container, and naturally cooling to room temperature to form white supramolecular gel;
2) drying the supramolecular gel: freezing the supramolecular gel obtained in the step 1) for 8-48 hours at the temperature of-5 to-50 ℃, and then drying in a vacuum environment;
3) high-temperature treatment of supramolecular gels: putting the supermolecule xerogel obtained in the step 2) into an atmosphere furnace, preserving the heat for 1-8 hours at the temperature of 1000-1800 ℃, and introducing argon or ammonia gas in the whole treatment process to finally obtain the boron nitride aerogel.
In the method for adjusting the properties of the boron nitride aerogel by utilizing the atmosphere, in the step 1), the total concentration of the prepared solution is set to be 20-60 mg/ml.
The method for adjusting the properties of the boron nitride aerogel by utilizing the atmosphere comprises the step of introducing different types of atmospheres at the high-temperature treatment stage corresponding to the step 3) to enable the obtained boron nitride aerogel to have different properties.
According to the method for adjusting the properties of the boron nitride aerogel by utilizing the atmosphere, in the step 3), when an argon atmosphere is selected, the obtained boron nitride aerogel is excellent in crystallinity, ordered in microstructure and 1-20 m in specific surface area2(ii)/g, exhibits significant hydrophilicity and brittleness; in contrast, when the ammonia gas atmosphere is selected, the obtained boron nitride aerogel has poorer crystallinity and more disordered microstructure, and the specific surface area of the boron nitride aerogel reaches 500m2Above/g, exhibits significant hydrophobicity and elasticity.
In the method for adjusting the properties of the boron nitride aerogel by utilizing the atmosphere, in the step 3), when the argon atmosphere is selected, the wetting angle of the obtained boron nitride aerogel to water is 0 degree; when an ammonia gas atmosphere is selected, the wetting angle of the obtained boron nitride aerogel to water is 100-150 degrees.
In the method for adjusting the properties of the boron nitride aerogel by using the atmosphere, in the step 3), the temperature of the high-temperature treatment stage is preferably set to be 1100-1500 ℃.
The design idea of the invention is as follows:
the melamine and the boric acid can be assembled in the solution through hydrogen bond action to form supermolecule gel, and the supermolecule wet gel can be converted into the boron nitride aerogel after being dried and treated at high temperature. During the high temperature treatment, the atmospheric environment may affect the conversion process of the supramolecular gel to boron nitride aerogel. Therefore, the boron nitride aerogel finally obtained can be made to exhibit different properties by changing the atmosphere.
The invention takes melamine and boric acid as molecular components to prepare supermolecule gel, the wet gel is frozen and dried to obtain supermolecule xerogel, and then the supermolecule xerogel is placed in a tubular atmosphere furnace for high-temperature treatment. And introducing different atmospheres in the high-temperature treatment stage to obtain the boron nitride aerogel with different properties.
The invention has the advantages and beneficial effects that:
1. the invention provides a method for adjusting the properties of boron nitride aerogel by utilizing atmosphere, which can effectively change the properties of the boron nitride aerogel by simply changing the atmosphere in a high-temperature conversion stage.
2. The method provided by the invention can effectively adjust the crystallinity, microstructure, wettability and mechanical properties of the boron nitride aerogel, and the boron nitride aerogel is convenient to adapt to different application scenes.
3. The method provided by the invention is simple and effective, is convenient to implement, is easy to realize the performance adjustment of the boron nitride aerogel, and lays a foundation for downstream application research.
4. The method provided by the invention can realize the integration of synthesis preparation and performance regulation and control, and avoids the intervention of post-processing means for realizing performance regulation. The whole process is simple and convenient, is easy to operate, and is convenient for realizing the mass synthesis of the boron nitride aerogel.
Drawings
FIG. 1 is a general flow chart of the use of an atmosphere to adjust the properties of boron nitride aerogels.
Fig. 2 is an XRD (X-ray diffraction) pattern of the boron nitride aerogel obtained under two atmosphere environments.
FIGS. 3a to 3b are transmission electron micrographs of two boron nitride aerogels. Wherein the sample number corresponding to FIG. 3a is BN-Ar-1400 deg.C (the right image is the high resolution photograph corresponding to the left image), and the sample number corresponding to FIG. 3b is BN-NH31400 deg.C (right picture is the corresponding high resolution photograph of the left picture).
Fig. 4a to 4b show the results of the wetting angle test of two boron nitride aerogels. Wherein the sample number corresponding to FIG. 4a is BN-Ar-1400 deg.C, and the sample number corresponding to FIG. 4b is BN-NH3-1400℃。
Fig. 5a to 5b show the nitrogen adsorption experiment results of two boron nitride aerogels. Wherein the sample number corresponding to FIG. 5a is BN-Ar-1100 deg.C, and the sample number corresponding to FIG. 5b is BN-NH3-1100℃。
FIGS. 6a to 6b show the mechanical property development of two boron nitride aerogelsIllustration. Wherein the sample number corresponding to FIG. 6a is BN-Ar-1100 deg.C (the upper graph is the relationship curve of displacement and force application, and the lower graph is the force application mode), and the sample number corresponding to FIG. 6b is BN-NH31100 deg.C (upper graph is the displacement versus force, lower graph is the force applied).
Detailed Description
As shown in fig. 1, the overall process of the present invention is as follows: the supermolecule gel is prepared by taking melamine (M) and boric acid (B) as molecular components, and can be converted into the boron nitride aerogel under the conditions of high-temperature treatment and different atmospheres after being frozen and dried. Changing the atmosphere used during the high temperature conversion process can significantly affect the properties of the resulting aerogel, such as: crystalline state, adsorption behavior, wettability, mechanical properties, etc.
The invention is further described below by means of specific examples.
Example 1
Firstly, 100ml of deionized water is measured and added into a glass beaker, and then melamine (M) and boric acid (B) are sequentially added according to the molar ratio of 1:6, so that the total concentration of the solution is 30mg/ml, specifically 0.76g of melamine and 2.24g of boric acid are taken; dissolving the materials in water bath at 80 deg.c and stirring for 6 hr, and cooling naturally in different containers at room temperature to observe the formation of white supermolecular gel; then, freezing the generated supermolecule wet gel for 20 hours at the temperature of minus 20 ℃, and immediately drying the gel in a vacuum environment; and finally, putting the dried gel into a tubular atmosphere furnace, and preserving the heat for 4 hours at 1100 ℃ to obtain the final Boron Nitride (BN) aerogel.
During the high-temperature treatment, two atmosphere environments are specifically selected:
firstly, marking a sample obtained under the condition as BN-Ar-1100 ℃ under an argon (Ar) environment;
② ammonia (NH)3) Ambient, the sample obtained under this condition was labeled BN-NH3-1100℃。
As shown in fig. 2, XRD patterns of BN aerogel obtained under two atmosphere environments. It can be seen that, although both aerogel samples show the characteristic peak of hexagonal boron nitride,the crystalline state of the polymer showed a distinct difference. The corresponding diffraction peak of the aerogel obtained in the argon environment is sharp, and the corresponding diffraction peak of the aerogel obtained in the ammonia environment is obviously wider, which indicates that the crystallinity of the aerogel is lower than that of the aerogel obtained in the argon environment. The crystallinity of these two samples can be further improved by treating them at 1400 ℃ where the corresponding samples are labeled BN-Ar-1400 ℃ and BN-NH, respectively3The crystallinity of the former is still better than that of the latter, as can be seen at-1400 ℃. BN-Ar-1400 ℃ and BN-NH under a transmission electron microscope3The two samples were observed at-1400 ℃ and a significant difference in microstructure was seen (see FIG. 3). In addition, examining the wettability of these two samples, it can be found that: the former has a contact angle of 0 DEG with water, and shows remarkable hydrophilicity; the latter has a contact angle with water of about 135 deg., showing a remarkable hydrophobicity (see fig. 4).
The results of the nitrogen adsorption experiment (see FIG. 5) show that BN-Ar-1100 ℃ and BN-NH3The adsorption isotherms corresponding to-1100 ℃ are of different types, and the specific surface areas calculated by the BET model are also significantly different, namely 9.038m2In terms of/g, the latter amount reaching 572.4m2(ii) in terms of/g. In addition, there is a clear difference in the mechanical properties of the two samples, the former showing significant brittleness and the latter showing significant elasticity, as shown in fig. 6.
Example 2
Firstly, weighing 200ml of deionized water, adding the deionized water into a glass beaker, and then sequentially adding melamine (M) and boric acid (B) according to a molar ratio of 1:6 to ensure that the total concentration of the solution is 40mg/ml, specifically, 2.03g of melamine and 5.97g of boric acid are taken; dissolving the materials in water bath at 90 deg.c and stirring for 1 hr, and cooling naturally in different containers at room temperature to observe the formation of white supermolecular gel; then, freezing the generated supermolecule wet gel at-30 ℃ for 12 hours, and immediately drying in a vacuum environment; and finally, putting the dried gel into a tubular atmosphere furnace, and preserving the heat for 4 hours at 1100 ℃ to obtain the final Boron Nitride (BN) aerogel. In the high-temperature treatment process, two atmosphere environments of argon and ammonia are specifically selected. At this time, the obtained boron nitride aerogel may exhibit a variation law similar to that in the previous embodiment in properties.
The results of the examples show that the present invention can adjust the properties of boron nitride aerogels using an atmosphere. The method is convenient to implement and easy for mass production, can realize performance adjustment in the synthesis preparation process, and avoids intervention post-processing means.
Claims (6)
1. A method for adjusting the properties of boron nitride aerogel by utilizing atmosphere is characterized in that the atmosphere used in a high-temperature conversion stage is changed to influence the properties of the obtained boron nitride aerogel, and the method comprises the following specific steps:
1) preparation of supramolecular gel: dissolving melamine and boric acid in a molar ratio of 1: 4-1: 8 in deionized water at 70-100 ℃, stirring for 0.1-10 hours to form a solution, pouring the solution into a container, and naturally cooling to room temperature to form white supramolecular gel;
2) drying the supramolecular gel: freezing the supramolecular gel obtained in the step 1) for 8-48 hours at the temperature of-5 to-50 ℃, and then drying in a vacuum environment;
3) high-temperature treatment of supramolecular gels: putting the supermolecule xerogel obtained in the step 2) into an atmosphere furnace, preserving the heat for 1-8 hours at the temperature of 1000-1800 ℃, and introducing argon or ammonia gas in the whole treatment process to finally obtain the boron nitride aerogel.
2. The method for adjusting the properties of the boron nitride aerogel by using the atmosphere according to claim 1, wherein in the step 1), the total concentration of the prepared solution is set to be 20-60 mg/ml.
3. The method for adjusting the properties of the boron nitride aerogel by utilizing the atmosphere according to claim 1, wherein different types of atmospheres are introduced at the high-temperature treatment stage corresponding to the step 3) to make the obtained boron nitride aerogel have different properties.
4. The use of atmosphere mediated nitridation of claim 1The method for preparing the boron aerogel is characterized in that in the step 3), when an argon atmosphere is selected, the obtained boron nitride aerogel is excellent in crystallinity, ordered in microstructure and 1-20 m in specific surface area2(ii)/g, exhibits significant hydrophilicity and brittleness; in contrast, when the ammonia gas atmosphere is selected, the obtained boron nitride aerogel has poorer crystallinity and more disordered microstructure, and the specific surface area of the boron nitride aerogel reaches 500m2Above/g, exhibits significant hydrophobicity and elasticity.
5. The method for adjusting the properties of the boron nitride aerogel by utilizing the atmosphere according to claim 3, wherein in the step 3), when an argon atmosphere is selected, the wetting angle of the obtained boron nitride aerogel to water is 0 degree; when an ammonia gas atmosphere is selected, the wetting angle of the obtained boron nitride aerogel to water is 100-150 degrees.
6. The method for conditioning the properties of boron nitride aerogel using an atmosphere according to claim 1, wherein in step 3), the temperature of the high-temperature treatment stage is preferably set to 1100 ℃ to 1500 ℃.
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- 2021-11-25 CN CN202111413519.9A patent/CN114180540A/en active Pending
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Application publication date: 20220315 |