CN111533093A - Preparation method of blocky boron nitride aerogel based on combination of freeze drying method and tubular furnace high-temperature heating method - Google Patents

Preparation method of blocky boron nitride aerogel based on combination of freeze drying method and tubular furnace high-temperature heating method Download PDF

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CN111533093A
CN111533093A CN202010477838.5A CN202010477838A CN111533093A CN 111533093 A CN111533093 A CN 111533093A CN 202010477838 A CN202010477838 A CN 202010477838A CN 111533093 A CN111533093 A CN 111533093A
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boron nitride
melamine
boric acid
freeze
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李玲
蒋祥倩
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Harbin Institute of Technology
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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
    • C01B21/068—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 silicon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0091—Preparation of aerogels, e.g. xerogels
    • 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
    • C01B21/068—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 silicon
    • C01B21/0687—After-treatment, e.g. grinding, purification
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0045—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by a process involving the formation of a sol or a gel, e.g. sol-gel or precipitation processes
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/10—Solid density

Abstract

The invention discloses a preparation method of blocky boron nitride aerogel based on combination of a freeze drying method and a tubular furnace high-temperature heating method, which comprises the following steps: firstly, weighing boric acid and melamine, and adding ultrapure water to form a melamine-boric acid hydrogel precursor; secondly, putting the melamine-boric acid hydrogel precursor into a water bath kettle for heat preservation to obtain a transparent solution, and then cooling to room temperature after ultrasonic treatment to obtain melamine-boric acid hydrogel; thirdly, freeze-drying the melamine-boric acid hydrogel to obtain massive boron nitride xerogel; and fourthly, introducing nitrogen-hydrogen mixed gas into the tubular furnace, putting the massive boron nitride xerogel on the corundum boat, pushing the corundum boat to a central high-temperature area of the tubular furnace for heating, and taking out the corundum boat after the corundum boat is cooled to room temperature to obtain the boron nitride aerogel. The massive boron nitride aerogel prepared by the invention has the advantages of excellent appearance, light weight, small density, simple and feasible method, simple and cheap experimental equipment and convenient experimental process.

Description

Preparation method of blocky boron nitride aerogel based on combination of freeze drying method and tubular furnace high-temperature heating method
Technical Field
The invention belongs to the field of preparation of boron nitride aerogel, relates to a preparation method of boron nitride aerogel, and particularly relates to a preparation method of blocky boron nitride aerogel based on combination of a freeze drying method and a tubular furnace high-temperature heating method.
Background
Aerogel (aerogel), a three-dimensional nanoporous material with ultra-high porosity, is the lightest condensed material among the current synthetic materials. The aerogel serving as a nano-pore super heat-insulating material has the characteristics of ultra-light weight and high thermal stability besides extremely low thermal conductivity, and has very wide application in the fields of industry, civil use, building, aerospace, military and the like. In the traditional industrial field: such as petrochemical industry, chemical industry, metallurgical industry and the like, pipelines, furnaces and other thermal equipment are ubiquitous, and the aerogel thermal insulation material is used for replacing the traditional thermal insulation material, so that the energy-saving effect is obvious. The nano-porous structure of the aerogel enables the aerogel to have excellent heat insulation performance, the heat conductivity of the aerogel is even lower than that of air, the heat conductivity of the air under the normal-temperature vacuum state is 0.026W/mK, the heat conductivity of the aerogel under the normal-temperature normal-pressure state is generally less than 0.02W/mK, and the heat conductivity of the aerogel under the vacuum state can be as low as 0.004W/mK. The conventional thermal insulation materials are porous structures, and it is the air that occupies a part of the volume of the solid material, thereby reducing the thermal conductivity of the whole material. The solid skeleton with extremely small content in the aerogel is also composed of nano particles, and the contact area of the solid skeleton is very small, so that the aerogel also has extremely small solid-state thermal conductivity. The fine nano-network structure of the aerogel effectively limits the propagation of local thermal excitation, and the nano-micropores inhibit the contribution of gas molecules to heat conduction.
Therefore, with the development of science and technology, more and more scientific researchers research novel aerogel materials, and the boron nitride aerogel has the advantages of stable chemical property, small size, unique porous structure, large specific surface area and the like as a novel nano material, and the excellent physical properties enable the aerogel to have wide application prospects in various fields such as aerospace, heat and sound insulation, adsorption catalysis, energy storage and the like.
Disclosure of Invention
In order to solve the problems of high preparation temperature, long time, high cost and the like of the boron nitride aerogel, the invention provides a preparation method of a blocky boron nitride aerogel based on the combination of a freeze drying method and a tubular furnace high-temperature heating method.
The purpose of the invention is realized by the following technical scheme:
a preparation method of blocky boron nitride aerogel based on combination of a freeze drying method and a tubular furnace high-temperature heating method comprises the following steps:
the method comprises the following steps: weighing a certain mass of boric acid and melamine by using an electronic balance, putting the boric acid and the melamine into a beaker, controlling the molar ratio of the boric acid to the melamine to be 1-3: 1 (such as: 1:1, 1.5:1, 2:1, 2.5:1 and 3:1), adding 200ml of ultrapure water, putting the mixture into a constant-temperature magnetic stirrer, stirring the mixture for 1-3 hours, fully and uniformly mixing the mixture to form a melamine-boric acid hydrogel precursor, and sealing the mouth of the beaker by using tin foil before carrying out magnetic stirring to isolate external environmental pollution;
step two: putting the melamine-boric acid hydrogel precursor obtained in the step one into a digital display constant-temperature water bath kettle, preserving the heat for 3-5 hours at 85-95 ℃ to obtain a transparent solution, then carrying out ultrasonic treatment for 0.5-1.5 hours, and cooling to room temperature (-25 ℃) to obtain melamine-boric acid hydrogel;
step three: putting the melamine-boric acid hydrogel obtained in the step two into a freeze dryer, and freeze-drying for 48-96 hours at-80 ℃ to obtain massive boron nitride xerogel;
step four: introducing nitrogen-hydrogen mixed gas (85% N) into the tube furnace2+15％H2) And putting the massive boron nitride xerogel obtained in the step three on a corundum boat, pushing the corundum boat to a central high-temperature area of a tubular furnace, setting the temperature of the tubular furnace to be 1000-1200 ℃, setting the heating time to be 1-3 hours, and taking out the corundum boat after the massive boron nitride xerogel is cooled to room temperature to obtain the boron nitride aerogel.
Analysis of reaction mechanism:
when the temperature of the tube furnace is heated to 100 ℃, boric acid loses one molecule of water to form metaboric acid HBO2Continuously heating to about 160 ℃ to obtain metaboric acid HBO2Conversion of molecules to pyroboric acid H by loss of one molecule of water2B4O7When the furnace temperature reaches above 400 ℃, all water molecules in the boric acid are removed completely to generate boron oxide B2O3Continued heating may produce elemental B atoms in the gaseous state while the melamine formsAmine molecules sublime at about 350 ℃ to form C3N4Molecule, then boron oxide by C3N4The C element in the boron nitride is reduced into simple substance B atoms, and the simple substance B atoms react with N atoms generated by the decomposition of melamine to generate the boron nitride. The gas overflows during the reaction process to form a porous structure of the boron nitride aerogel, and the chemical equation of the reaction is as follows:
H3BO3(s)→HBO2+H2O(g)；
4HBO2(s)→H2B4O7+H2O(g)；
H2B4O7(s)→2B2O3(s)+H2O(g)；
C3N3(NH2)3(s)→C3N4(s)+2NH3(g)；
B2O3(s)+3C+N2→2BN+3CO(g)。
compared with the prior art, the invention has the following advantages:
1. the massive boron nitride aerogel prepared by the invention has the advantages of excellent appearance, light weight and small density.
2. The method is simple and easy to implement, the used experimental equipment is simple and cheap, and the experimental process is convenient.
3. Compared with the traditional element substitution method for synthesizing the boron nitride aerogel, the required temperature is low (less than 1300 ℃), and compared with the traditional template substitution method for preparing the boron nitride aerogel, the carbon aerogel template does not need to be prepared, so that the cost is greatly reduced.
Drawings
FIG. 1 is a physical diagram of a bulk boron nitride aerogel prepared in example 1;
FIG. 2 is a photograph of a block-shaped boron nitride aerogel prepared in example 1 placed on the leaves of a plant;
FIG. 3 is an X-ray diffraction (XRD) spectrum of the bulk boron nitride aerogel prepared in example 1;
FIG. 4 is a Scanning Electron Microscope (SEM) image of a bulk boron nitride aerogel prepared in example 1;
FIG. 5 is a Transmission Electron Microscope (TEM) image of a bulk boron nitride aerogel prepared in example 1;
fig. 6 is a High Resolution Transmission Electron Microscope (HRTEM) image of the bulk boron nitride aerogel prepared in example 1.
Detailed Description
The technical solution of the present invention is further described below with reference to the accompanying drawings, but not limited thereto, and any modification or equivalent replacement of the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention shall be covered by the protection scope of the present invention.
Example 1:
in this embodiment, the preparation method of the bulk boron nitride aerogel is as follows:
the method comprises the following steps: weighing 7.2g of boric acid and 5g of melamine by using an electronic balance, putting the boric acid and the melamine into a beaker, adding 100ml of deionized water, putting the beaker on a constant-temperature magnetic stirrer, and stirring the mixture for 2 hours to ensure that the mixture is fully and uniformly mixed to form a melamine-boric acid hydrogel precursor, and sealing the opening of the beaker by using tinfoil before magnetic stirring to isolate external environmental pollution.
Step two: and (3) putting the melamine-boric acid hydrogel in the beaker into a digital display constant temperature water bath kettle, keeping the temperature for 4 hours at 90 ℃ to obtain a transparent solution, then carrying out ultrasonic treatment for 1 hour, and cooling to room temperature (-25 ℃) to obtain white hydrogel.
Step three: and (3) putting the melamine-boric acid hydrogel in the beaker into a freeze dryer, and freeze-drying for 72 hours at the temperature of minus 80 ℃ to obtain the massive boron nitride xerogel.
Step four: introducing nitrogen-hydrogen mixed gas (85% N) into the tube furnace2+15％H2) Putting the boron nitride xerogel on a corundum boat, pushing the corundum boat to a central high-temperature area of a tube furnace, and setting the temperature of the tube furnace as stage one: heating to 1100 ℃, and performing stage two: constant temperature at 1100 ℃ for 3 hours, stage three: naturally cooling to room temperature, and taking out after cooling to room temperature to obtain the boron nitride aerogel.
FIG. 1 is a physical diagram of a bulk boron nitride aerogel prepared in example 1; FIG. 2 is a schematic view ofPhotograph of the block-shaped boron nitride aerogel prepared in example 1 placed on the leaf of a plant, the true density of the boron nitride aerogel was only 0.028g/cm3。
FIG. 3 is an X-ray diffraction (XRD) spectrum of the bulk boron nitride aerogel and hexagonal boron nitride material (h-BN) prepared in example 1. From the XRD patterns, it can be seen that the boron nitride aerogel has two very strong diffraction peaks measured at 2 θ 26.55 and 2 θ 41.82, which represent the (002) and (100) crystal planes of boron nitride. In addition, the diffraction peaks of the (002) and (100) crystal planes of the boron nitride aerogel are perfectly matched at the same angle compared to pure h-BN. This further illustrates that the product of this experiment is h-BN. In addition, the (002) diffraction peak of the boron nitride aerogel is narrow and strong, indicating that the crystallinity of the BN aerogel is increasing.
FIG. 4 is a Scanning Electron Microscope (SEM) image of a bulk boron nitride aerogel prepared in example 1; fig. 5 is a Transmission Electron Microscope (TEM) image of the bulk boron nitride aerogel prepared in example 1. As can be seen from FIG. 4, the prepared boron nitride aerogel has high yield, is in a nano-belt-shaped cross disordered arrangement and random orientation, and has a length of about 50-200 μm and a width of about 100 nm-3 μm. As can be seen in a Transmission Electron Microscope (TEM) of FIG. 5, the prepared boron nitride aerogel has good morphology and is a straight long-strip structure. The staggered lattice fringes can be clearly seen in the high resolution TEM image (HRTEM) of fig. 6. The long belt shape and the staggered lattice stripe shape of the boron nitride aerogel cause the boron nitride aerogel to have a large specific surface area.
Comparative example 1:
this comparative example differs from example 1 in that: the mass of boric acid in step one was 2.9g, 4.3g, 5.7g, 7.2g and 8.6g, respectively. The other steps were the same as in example 1.
The boron nitride aerogel prepared by the comparative example is found to have excellent morphology when the molar ratio of boric acid to melamine is 2.5:1, and the straight staggered boron nitride nanobelt structure can be observed under a Scanning Electron Microscope (SEM) and a Transmission Electron Microscope (TEM).
Comparative example 2:
this comparative example differs from example 1 in that: and in the third step, the freeze drying of the freeze dryer is set to be 48 hours, 72 hours and 96 hours respectively, and a control experiment for forming the massive boron nitride xerogel is obtained. The other steps were the same as in example 1.
The boron nitride aerogel prepared by the embodiment is found that the frozen boron nitride xerogel with stable shape after being frozen by the freeze dryer within 72 hours, while the boron nitride xerogel with 48 hours of freeze drying has more water content, which is not beneficial for subsequent experiments, and the boron nitride xerogel with 96 hours of freeze drying is very crisp, has poor compactness and is not easy to form.
Comparative example 3:
this comparative example differs from example 1 in that: heating temperatures of the tubular furnace in the four steps were set to 1000 deg.C, 1100 deg.C and 1200 deg.C, respectively, and other steps were the same as in example 1.
The boron nitride aerogel prepared by the comparative example was found to be pure white in color when the heating temperature of the tube furnace was 1100 ℃, while the boron nitride aerogel prepared at the temperature of 1200 ℃ was yellowish in color. The bulk boron nitride aerogel prepared at 1000 ℃ has higher density, and analysis shows that the porous structure of the boron nitride aerogel is not completely formed due to too low temperature.
Comparative example 4:
this comparative example differs from example 1 in that: heating time of the tube furnace in the four steps was set to 1 hour, 2 hours, and 3 hours, and other steps were the same as in example 1.
The boron nitride aerogel prepared by the comparative example was found to have the smallest density and the lightest weight when the tube furnace was heated for 3 hours.

Claims (10)

1. A preparation method of blocky boron nitride aerogel based on combination of a freeze drying method and a tubular furnace high-temperature heating method is characterized by comprising the following steps:
the method comprises the following steps: weighing a certain mass of boric acid and melamine, putting the boric acid and the melamine into a beaker, controlling the molar ratio of the boric acid to the melamine to be 1-3: 1, adding 200ml of ultrapure water, and then magnetically stirring for 1-3 hours to fully and uniformly mix the boric acid and the melamine to form a melamine-boric acid hydrogel precursor;
step two: putting the melamine-boric acid hydrogel precursor obtained in the step one into a water bath kettle, preserving heat for 3-5 hours at 85-95 ℃ to obtain a transparent solution, then carrying out ultrasonic treatment for 0.5-1.5 hours, and cooling to room temperature to obtain melamine-boric acid hydrogel;
step three: putting the melamine-boric acid hydrogel obtained in the step two into a freeze dryer, and freeze-drying for 48-96 hours at-80 ℃ to obtain massive boron nitride xerogel;
step four: and (3) introducing nitrogen-hydrogen mixed gas into the tubular furnace, placing the massive boron nitride xerogel obtained in the step three on a corundum boat, pushing the corundum boat to a central high-temperature region of the tubular furnace, setting the temperature of the tubular furnace to be 1000-1200 ℃, setting the heating time to be 1-3 hours, and taking out the corundum boat after the tubular furnace is cooled to room temperature to obtain the boron nitride aerogel.
2. The method for preparing the massive boron nitride aerogel based on the combination of the freeze-drying method and the tube furnace high-temperature heating method according to claim 1, wherein the molar ratio of the boric acid to the melamine is 1:1, 1.5:1, 2:1, 2.5:1 or 3: 1.
3. The method for preparing the blocky boron nitride aerogel based on the combination of the freeze-drying method and the tube furnace high-temperature heating method according to claim 1, wherein the opening of the beaker is sealed by tinfoil before the magnetic stirring, so that the outside environment pollution is isolated.
4. The method for preparing the block boron nitride aerogel based on the combination of the freeze-drying method and the tube furnace high-temperature heating method according to claim 1, wherein the magnetic stirring time is 2 hours.
5. The method for preparing the blocky boron nitride aerogel based on the combination of the freeze drying method and the tube furnace high-temperature heating method according to claim 1, wherein the temperature of the water bath is 90 ℃ and the time is 4 hours.
6. The method for preparing the massive boron nitride aerogel based on the combination of the freeze-drying method and the tube furnace high-temperature heating method according to claim 1, wherein the ultrasonic treatment time is 1 h.
7. The method for preparing the block boron nitride aerogel based on the combination of the freeze-drying method and the tube furnace high-temperature heating method according to claim 1, wherein the freeze-drying time is 48 hours, 72 hours or 96 hours.
8. The method for preparing the block boron nitride aerogel based on the combination of the freeze-drying method and the tube furnace high-temperature heating method according to claim 1, wherein the heating temperature of the tube furnace is 1000 ℃, 1100 ℃ or 1200 ℃.
9. The method for preparing the block boron nitride aerogel based on the combination of the freeze-drying method and the tube furnace high-temperature heating method according to claim 1, wherein the heating time of the tube furnace is 1 hour, 2 hours or 3 hours.
10. The method for preparing the massive boron nitride aerogel based on the combination of the freeze-drying method and the tube furnace high-temperature heating method as claimed in claim 1, wherein N is contained in the nitrogen-hydrogen mixed gas2In an amount of 85% by volume, H2The content of (b) is 15% by volume.
CN202010477838.5A 2020-05-29 2020-05-29 Preparation method of blocky boron nitride aerogel based on combination of freeze drying method and tubular furnace high-temperature heating method Pending CN111533093A (en)

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Publication number Priority date Publication date Assignee Title
CN112811419A (en) * 2021-03-29 2021-05-18 宇荣(江苏)新材料科技有限公司 Low-cost preparation process of carbon aerogel and carbon aerogel
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CN113307238A (en) * 2021-04-26 2021-08-27 中国科学院金属研究所 Method for adjusting boron nitride nanobelt microstructure by using temperature-mediated assembly strategy
CN115260995A (en) * 2022-07-22 2022-11-01 中国地质大学（武汉） Double-network heat-conducting porous aerogel energy storage material and preparation method and application thereof
CN115196988A (en) * 2022-07-29 2022-10-18 陕西科技大学 Nitride nanobelt modified carbon/carbon composite material and preparation method thereof
CN116425554A (en) * 2023-04-27 2023-07-14 郑州大学 Boron nitride@silicon dioxide composite ceramic aerogel and preparation method thereof

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