CN115611635B - Boron nitride fiber and preparation method and application thereof - Google Patents
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Abstract
The invention belongs to the technical field of ceramic fiber preparation, and discloses a boron nitride fiber, a preparation method and application thereof, wherein the preparation method comprises the following steps: winding boron oxide fibers on an insulating medium in a DBD reactor, and treating according to the following process schedule: the first stage is as follows: in the ammonia atmosphere, heating the temperature of the DBD reactor from room temperature to 300 +/-50 ℃, controlling the DBD reactor to discharge and preserving the heat for 30-120min, continuously heating the DBD reactor to 600 +/-50 ℃, and preserving the heat for 30-120min; and a second stage: and under the nitrogen atmosphere, continuously heating the DBD reactor to 1000 +/-50 ℃, preserving the heat for 30-180min, and cooling to room temperature. The preparation method of the invention can greatly reduce the reaction temperature and accelerate the reaction rate, and the prepared boron nitride fiber has higher purity.
Description
Technical Field
The invention belongs to the technical field of ceramic fiber preparation, and particularly relates to a boron nitride fiber and a preparation method and application thereof.
Background
The novel boron nitride-based (h-BN) ceramic fiber is a known wave-transparent material reinforcing agent with the highest temperature resistance (> 2000 ℃), is expected to meet the use requirements of an aircraft on a heat wave-transparent material in a high-speed and long-time flying environment, and is the best scheme for preparing a new-generation missile radome high-temperature-resistant low-ablation wave-transparent material reinforcing body.
In the prior art, boron nitride is mainly prepared by reacting boron oxide with ammonia gas, the process is a gas-solid reaction process, and the activity of a reaction system is improved by high reaction temperature and long reaction time for obtaining high-purity boron nitride fibers due to low reaction activity of the ammonia gas. Therefore, the existing method for preparing the boron nitride fiber has the defects of high reaction temperature, long time, slow speed and low purity, and the ammonia gas has higher corrosivity to reaction equipment at high temperature, so that the equipment is easily damaged.
Disclosure of Invention
In order to solve the defects of the prior art, the invention discloses a preparation method of boron nitride fiber, which comprises the following specific scheme:
winding boron oxide fibers on an insulating medium in a DBD reactor, and treating according to the following process schedule:
the first stage is as follows: in the atmosphere of ammonia gas, heating the temperature of the DBD reactor from room temperature to 300 +/-50 ℃, preserving the temperature for 30-120min, continuously heating the DBD reactor to 600 +/-50 ℃, and preserving the temperature for 30-120min, wherein the DBD reactor is controlled to discharge in the process of heating to 300 +/-50 ℃ until the first stage is finished;
and a second stage: and under the nitrogen atmosphere, continuously heating the DBD reactor to 1000 +/-50 ℃, preserving the heat for 30-180min, and cooling to room temperature.
In the first stage, the DBD technology, namely the dielectric barrier plasma discharge technology, is adopted to activate ammonia gas into NHx free radicals and electrons, namely the ammonia gas with lower activity is converted into NHx free radicals with higher activity to participate in the reaction, and the temperature required by the reaction is greatly reduced due to the improvement of the activity of the substances participating in the reaction, compared with the prior art that the temperature required by the reaction of the ammonia gas and boron oxide fibers needs to reach more than 800 ℃, the temperature of the invention is 600 +/-50 ℃, and NH is carried out at the temperature of more than 800 DEG C X The free radicals can react with the boron oxide fiber to generate the boron nitride fiber; meanwhile, the NHx free radical has higher activity, so that the reaction rate is accelerated, and the purity of the generated boron nitride is higher.
However, because the reaction temperature in the first stage is low, the generated boron nitride is amorphous boron nitride, the crystal has defects and poor crystallinity, and further temperature rise is needed to convert the amorphous boron nitride into hexagonal boron nitride which is high temperature resistant and water washing resistant.
In the prior art, the reaction temperature of ammonia and boron oxide is high (the reaction temperature of ammonia and boron oxide is required to be over 800 ℃, the reaction temperature in the prior art is about 1000-1100 ℃, if boron oxide which does not participate in the reaction is volatilized from generated boron nitride, the required reaction temperature is required to be increased to over 1400 ℃), the ammonia and the boron oxide react to generate water, and the generated water reacts with the ammonia to generate corrosive ammonia water.
In the first stage of the invention, ammonia gas is activated into free radicals at low temperature to participate in the reaction, and the activity of the metal material of the metal equipment is lower, and the ammonia water basically does not corrode the metal material.
Further, the discharge voltage of the DBD reactor is 300V +/-100V, the discharge time is that the discharge is continued until the first stage is finished, or the discharge is performed every 5-10min, and the discharge lasts for 5-10min each time until the first stage is finished.
Further, the insulating medium is a silicon nitride ceramic cylinder or an alumina ceramic cylinder. Experiments have shown that silicon nitride ceramic cylinders are less prone to breakdown when used as an insulating medium than alumina ceramic cylinders.
Further, the insulating medium is a silicon nitride ceramic cylinder, the low-voltage electrode of the DBD reactor is located in the silicon nitride ceramic cylinder, and the high-voltage electrode of the DBD reactor is located outside the silicon nitride ceramic cylinder.
Further, in the first stage, nitrogen is introduced into the DBD reactor as a shielding gas.
Further, the specific temperature rise process in the first stage is as follows: heating from room temperature to 150 + -50 deg.C at a rate of 0.1-5 deg.C/min, maintaining for 30-180min, heating to 300 + -50 deg.C at a rate of 0.1-5 deg.C/min, maintaining for 30-120min, heating to 600 + -50 deg.C at a rate of 0.1-5 deg.C/min, and maintaining for 30-120min.
Further, the specific temperature rise process of the second stage is as follows: heating from 600 + -50 deg.C to 1000 + -50 deg.C at a rate of 1-10 deg.C/min, maintaining for 30-180min, and naturally cooling to room temperature.
The invention also discloses a boron nitride fiber prepared by any one of the preparation methods.
The invention also discloses application of any one of the boron nitride fibers in the technical field of ceramic fiber materials. The boron nitride fiber can be applied to preparation of high-temperature-resistant low-ablation wave-transparent materials, battery diaphragms, high-heat-conducting materials and the like.
Compared with the prior art, the invention has the beneficial effects that: the invention adopts DBD (dielectric barrier plasma discharge) technology to activate ammonia gas into NHx free radicals and electrons, NH X The free radicals can react with the boron oxide fiber to generate boron nitride fiber in situ due to NH X The activity of free radicals is high, the reaction temperature can be greatly reduced, the reaction rate is accelerated, and the purity of the prepared boron nitride fiber is high; the invention can effectively reduce the corrosion to reaction equipment by dividing the process system into two stages, and particularly, in the first stage, ammonia gas is activated into NH at lower temperature X The free radicals react with the boron oxide fibers to generate amorphous boron nitride fibers; in the second stage, the amorphous boron nitride is directly converted into the hexagonal boron nitride with good stability in the nitrogen atmosphere and at a higher temperature without ammonia atmosphere, so that the stability of the generated boron nitride fiber is ensuredAnd meanwhile, the corrosion of ammonia gas to reaction equipment in a high-temperature environment is also avoided. The fiber diameter of the boron nitride fiber prepared by the invention is 7 +/-1 mu m, the nitrogen content is 55.5-56.4 percent, and the monofilament strength of the fiber is 850 +/-150 MPa.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Winding boron oxide fibers on a silicon nitride ceramic cylinder in a DBD reactor, wherein a low-voltage electrode of the DBD reactor is positioned in the silicon nitride ceramic cylinder, a high-voltage electrode is positioned outside the silicon nitride ceramic cylinder, and treating according to the following process system:
the first stage is as follows: and introducing ammonia gas into the DBD reactor, introducing nitrogen gas serving as protective gas, heating from room temperature to 100 ℃ at the speed of 0.1 ℃/min, preserving heat for 180min, heating to 250 ℃ at the speed of 0.1 ℃/min, preserving heat for 120min, heating to 550 ℃ at the speed of 0.1 ℃/min, and preserving heat for 120min, wherein when the temperature in the DBD reactor reaches 250 ℃, the DBD reactor is controlled to discharge, the discharge voltage is 200V, and the discharge time is continuous discharge until the first stage is finished.
And a second stage: stopping introducing ammonia gas into the DBD reactor, introducing nitrogen gas into the DBD reactor, ensuring that the atmosphere in the DBD reactor is nitrogen atmosphere, heating from 550 ℃ to 950 ℃ at the speed of 1 ℃/min, preserving heat for 180min, and naturally cooling to room temperature.
Comparative example 1
Comparative example 1 is different from example 1 only in that the DBD reactor of comparative example 1 is not discharge-treated and other steps are the same as example 1.
The properties of the boron nitride fibers prepared in example 1 and comparative example 1 are shown in table 1:
TABLE 1
Example 2
Winding boron oxide fibers on an alumina ceramic cylinder in a DBD reactor, wherein a low-voltage electrode of the DBD reactor is positioned in the alumina ceramic cylinder, a high-voltage electrode is positioned outside the alumina ceramic cylinder, and treating according to the following process system:
the first stage is as follows: and introducing ammonia gas into the DBD reactor, introducing nitrogen gas serving as protective gas, heating from room temperature to 200 ℃ at the speed of 5 ℃/min, preserving heat for 30min, heating to 350 ℃ at the speed of 5 ℃/min, preserving heat for 30min, heating to 650 ℃ at the speed of 5 ℃/min, preserving heat for 30min, controlling the DBD reactor to discharge when the temperature in the DBD reactor reaches 350 ℃, wherein the discharge voltage is 400V, the discharge time is that electricity is discharged every 5min, and the discharge lasts for 5min each time until the first stage is finished.
And a second stage: stopping introducing ammonia gas into the DBD reactor, introducing nitrogen gas into the DBD reactor, ensuring that the atmosphere in the DBD reactor is nitrogen atmosphere, heating from 650 ℃ to 1050 ℃ at the speed of 10 ℃/min, preserving heat for 30min, and naturally cooling to room temperature.
Comparative example 2
Comparative example 2 is different from example 2 only in that the DBD reactor of comparative example 2 is not discharge-treated and other steps are the same as example 2.
The properties of the boron nitride fibers prepared in example 2 and comparative example 2 are shown in table 2:
TABLE 2
Example 3
Winding boron oxide fibers on a silicon nitride ceramic cylinder in a DBD reactor, wherein a low-voltage electrode of the DBD reactor is positioned in the silicon nitride ceramic cylinder, a high-voltage electrode is positioned outside the silicon nitride ceramic cylinder, and treating according to the following process system:
the first stage is as follows: and introducing ammonia gas into the DBD reactor, introducing nitrogen gas serving as protective gas, heating from room temperature to 150 ℃ at the speed of 2 ℃/min, preserving heat for 100min, heating to 300 ℃ at the speed of 2 ℃/min, preserving heat for 80min, heating to 600 ℃ at the speed of 2 ℃/min, preserving heat for 80min, controlling the DBD reactor to discharge when the temperature in the DBD reactor reaches 300 ℃, wherein the discharge voltage is 300V, the discharge time is that electricity is discharged every 10min, and the discharge lasts for 10min each time until the first stage is finished.
And a second stage: stopping introducing ammonia gas into the DBD reactor, introducing nitrogen gas into the DBD reactor, ensuring that the atmosphere in the DBD reactor is a nitrogen atmosphere, heating from 600 ℃ to 1000 ℃ at the speed of 5 ℃/min, preserving heat for 100min, and naturally cooling to room temperature.
Comparative example 3
Comparative example 3 is different from example 3 only in that the DBD reactor of comparative example 3 is not discharge-treated and other steps are the same as example 3.
The properties of the boron nitride fibers prepared in example 3 and comparative example 3 are shown in table 3:
TABLE 3
The term "average" in "average monofilament diameter" and "average monofilament tensile strength" measured in examples 1 to 3 and comparative examples 1 to 3 means that a section of 4 to 5cm of a fiber bundle is randomly cut out from a prepared boron nitride fiber, 25 to 30 boron nitride fiber monofilaments are randomly extracted from the fiber bundle, the diameter and the tensile strength of each boron nitride fiber are respectively detected, invalid data are discarded, the number of valid data is ensured to be more than or equal to 20, and then the average value is obtained. See GJB1871 for the test method for average monofilament tensile strength.
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art may still modify the technical solutions described in the foregoing embodiments, or may equally substitute some or all of the technical features; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.
Claims (8)
1. A preparation method of boron nitride fiber is characterized by comprising the following steps:
winding boron oxide fibers on an insulating medium in a DBD reactor, and treating according to the following process schedule:
the first stage is as follows: in the ammonia atmosphere, heating the temperature of the DBD reactor from room temperature to 300 +/-50 ℃, preserving the heat for 30-120min, continuously heating the DBD reactor to 600 +/-50 ℃, preserving the heat for 30-120min, wherein the DBD reactor is controlled to discharge in the process of heating to 300 +/-50 ℃ until the first stage is finished;
and a second stage: under the nitrogen atmosphere, continuously heating the DBD reactor to 1000 +/-50 ℃, preserving the heat for 30-180min, cooling to room temperature,
the specific temperature rise process of the first stage is as follows:
heating from room temperature to 150 + -50 deg.C at a rate of 0.1-5 deg.C/min, maintaining for 30-180min, heating to 300 + -50 deg.C at a rate of 0.1-5 deg.C/min, maintaining for 30-120min, heating to 600 + -50 deg.C at a rate of 0.1-5 deg.C/min, and maintaining for 30-120min.
2. The method for producing boron nitride fiber according to claim 1,
the discharge voltage of the DBD reactor is 300V +/-100V, the discharge time is that the discharge is continued until the first stage is finished, or the discharge is performed every 5-10min, and the discharge lasts for 5-10min each time until the first stage is finished.
3. The method of claim 1, wherein the insulating medium is a silicon nitride ceramic cylinder or an alumina ceramic cylinder.
4. The method of claim 1, wherein the insulating medium is a silicon nitride ceramic cylinder,
and a low-voltage electrode of the DBD reactor is positioned in the silicon nitride ceramic cylinder, and a high-voltage electrode of the DBD reactor is positioned outside the silicon nitride ceramic cylinder.
5. The method for preparing boron nitride fiber according to claim 1, wherein nitrogen is introduced into the DBD reactor as a shielding gas in the first stage.
6. The method for preparing boron nitride fiber according to claim 1, wherein the specific temperature rise process of the second stage is as follows:
heating from 600 + -50 deg.C to 1000 + -50 deg.C at a rate of 1-10 deg.C/min, maintaining for 30-180min, and naturally cooling to room temperature.
7. A boron nitride fiber produced by the method for producing a boron nitride fiber according to any one of claims 1 to 6.
8. Use of the boron nitride fiber of claim 7 in the technical field of ceramic fiber materials.
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