CN115385705B - Boron nitride fiber mat and preparation method thereof - Google Patents
Boron nitride fiber mat and preparation method thereof Download PDFInfo
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- CN115385705B CN115385705B CN202211215367.6A CN202211215367A CN115385705B CN 115385705 B CN115385705 B CN 115385705B CN 202211215367 A CN202211215367 A CN 202211215367A CN 115385705 B CN115385705 B CN 115385705B
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
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- C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
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Abstract
The invention discloses a boron nitride fiber mat and a preparation method thereof. The preparation method comprises the following steps: (1) Chopping, mixing and lapping the boron nitride fibers and the boron nitride precursor fibers to obtain a fiber felt blank; (2) Carrying out hot pressing treatment on the fiber mat blank to obtain a fiber mat preform; (3) And nitriding the fiber mat preform to obtain the boron nitride fiber mat. The boron nitride fiber felt prepared by the invention has particularly good high temperature resistance, and can still maintain higher mechanical strength under the high temperature condition.
Description
Technical Field
The invention belongs to the technical field of ceramic fiber materials, and particularly relates to a boron nitride fiber felt and a preparation method thereof.
Background
The most widely used fiber mats are glass fiber mats, which typically require the addition of an organic binder to be reinforced, and are not applicable in locations exceeding 600 c due to pyrolysis of the organic binder and melting of the glass fibers exceeding 600 c.
The air atmosphere of the boron nitride fiber can resist the high temperature of 900 ℃, and the inert atmosphere can resist the high temperature of 2000 ℃, but the common organic binder can be gradually decomposed and carbonized to lose the binding force, so that the fiber felt loses the mechanical strength.
Disclosure of Invention
Aiming at the problems, the invention provides the boron nitride fiber felt and the preparation method thereof, and the fiber felt prepared by the invention has particularly good high temperature resistance and can still maintain higher mechanical strength at high temperature.
The invention provides a preparation method of a boron nitride fiber mat, which comprises the following steps: (1) Chopping, mixing and lapping the boron nitride fibers and the boron nitride precursor fibers to obtain a fiber felt blank; (2) Carrying out hot pressing treatment on the fiber mat blank to obtain a fiber mat preform; (3) And nitriding the fiber mat preform to obtain the boron nitride fiber mat.
Preferably, the boron nitride precursor fiber is prepared by the following method: boron trichloride and methylamine are used as raw materials to prepare a boron nitride precursor, and the boron nitride precursor is heated and melted and then drawn into the wire.
Preferably, the boron nitride fibers and the boron nitride precursor fibers are mixed in a weight ratio of 1:1-5.
Preferably, the boron nitride fibers and boron nitride precursor fibers are chopped to 3-20mm.
Preferably, the method specifically comprises the following steps: chopping boron nitride fibers; chopping boron nitride precursor fibers; adding the chopped boron nitride fibers and boron nitride precursor fibers into a fiber settling chamber, dispersing and mixing uniformly under the blowing of dry air, and settling on a mesh belt to obtain the fiber felt blank.
Preferably, in the step (2), the pressure is 0.01-0.1MPa and the temperature is 150-300 ℃ during the hot pressing treatment.
Preferably, in the step (2), a heat press roller is used for the heat press treatment.
Preferably, in the step (3), the temperature is 950-1050 ℃ during the nitriding treatment.
Preferably, in the step (3), the atmosphere at the nitriding treatment is ammonia gas and nitrogen gas.
The invention also provides the boron nitride fiber felt prepared by the method.
Compared with the prior art, the invention has the following beneficial effects:
(1) The boron nitride fiber felt prepared by the invention has the characteristics of high temperature resistance, high dielectric property, low heat conduction, corrosion resistance and the like, can be used for heat preservation treatment of high-temperature equipment, can also be used for reinforcing alloy and high-temperature filter materials, and is an ideal material for aerospace, and the composite material prepared by the boron nitride fiber felt has good wave-transmitting performance.
(2) The boron nitride fiber felt bonded by the boron nitride is prepared by dry forming, has simple and convenient process, excellent performance and wide application range, particularly has particularly good high temperature resistance, and can still maintain higher mechanical strength at high temperature.
(3) The boron nitride precursor is uniformly mixed with the boron nitride fiber in a fiber form, the precursor fiber is softened and bonded with the boron nitride fiber at a high temperature under the condition of applying a certain pressure, and finally the boron nitride precursor fiber is converted into the boron nitride fiber through nitriding treatment, so that the boron nitride fiber felt with higher mechanical strength under the condition of high temperature is finally formed.
Drawings
Fig. 1 is a boron nitride fiber mat prepared in example 1 of the present invention.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a preparation method of a boron nitride fiber mat, which comprises the following steps:
(1) And (3) chopping, mixing and lapping the boron nitride fibers and the boron nitride precursor fibers to obtain the fiber felt blank.
Specifically, chopping boron nitride fibers into 3-20mm; chopping boron nitride precursor fiber into 3-20mm in a constant temperature and humidity environment (the temperature is controlled to be 25+/-2 ℃ and the humidity is controlled to be 8+/-4 percent); adding the chopped boron nitride fibers and boron nitride precursor fibers into a fiber settling chamber according to the weight ratio of 1: (1-5), dispersing and mixing uniformly under the blowing of dry air, and settling on a mesh belt to obtain the fiber felt blank.
Wherein the boron nitride precursor fiber is prepared by the following method: boron trichloride and methylamine are used as raw materials, toluene is used as a solvent to prepare a boron nitride precursor, and the boron nitride precursor is heated and melted and then drawn under a constant temperature and humidity environment (the temperature is controlled to be 25+/-2 ℃ and the humidity is controlled to be 8+/-4%).
(2) And carrying out hot pressing treatment on the fiber mat blank to obtain a fiber mat preform.
Specifically, the fiber mat blank is subjected to hot pressing treatment by a hot pressing roller, the pressure is controlled to be 0.01-0.1MPa, and the temperature is controlled to be 150-300 ℃, so that boron nitride precursor fibers in the fiber mat blank are softened, and boron nitride fibers are bonded to form a mat, and then the fiber mat preform is obtained.
(3) And (3) sending the fiber mat preform into a high-temperature furnace to carry out nitriding treatment at 950-1050 ℃ in an ammonia gas and nitrogen gas atmosphere, so that the components of the boron nitride precursor fibers are converted (namely, the boron nitride precursor is converted into boron nitride), and the boron nitride combined boron nitride fiber mat is obtained.
The invention also provides the boron nitride fiber felt prepared by the method.
Example 1
The embodiment provides a preparation method of a boron nitride fiber mat, which comprises the following steps:
(1) And (3) chopping, mixing and lapping the boron nitride fibers and the boron nitride precursor fibers to obtain the fiber felt blank.
Specifically, chopping boron nitride fibers into 3-20mm; chopping boron nitride precursor fiber into 3-20mm in a constant temperature and humidity environment with the temperature of 25 ℃ and the humidity of 8%; adding the chopped boron nitride fibers and boron nitride precursor fibers into a fiber settling chamber according to the weight ratio of 1:3, dispersing and mixing uniformly under the blowing of dry air, and settling on a mesh belt to obtain the fiber felt blank.
Wherein the boron nitride precursor fiber is prepared by the following method: boron trichloride and methylamine are used as raw materials, toluene is used as a solvent to prepare a boron nitride precursor, and the boron nitride precursor is heated and melted and then drawn under the constant temperature and humidity environment with the temperature of 25 ℃ and the humidity of 8 percent to obtain the boron nitride precursor.
(2) And carrying out hot pressing treatment on the fiber mat blank to obtain a fiber mat preform.
Specifically, the fiber mat blank is subjected to hot pressing treatment through a hot pressing roller, the pressure is controlled to be 0.05MPa, the temperature is controlled to be 220 ℃, boron nitride precursor fibers in the fiber mat blank are softened, and boron nitride fibers are bonded to form a mat, so that the fiber mat preform is obtained.
(3) And (3) sending the fiber mat preform into a high-temperature furnace to carry out nitriding treatment at 1000 ℃ in an ammonia gas and nitrogen gas atmosphere, so that the components of the boron nitride precursor fibers are converted (namely, the boron nitride precursor is converted into boron nitride), and the boron nitride combined boron nitride fiber mat is obtained.
The embodiment also provides the boron nitride fiber mat prepared by the method.
Example 2
The embodiment provides a preparation method of a boron nitride fiber mat, which comprises the following steps:
(1) And (3) chopping, mixing and lapping the boron nitride fibers and the boron nitride precursor fibers to obtain the fiber felt blank.
Specifically, chopping boron nitride fibers into 3-20mm; chopping boron nitride precursor fiber into 3-20mm in a constant temperature and constant humidity environment; adding the chopped boron nitride fibers and boron nitride precursor fibers into a fiber settling chamber according to the weight ratio of 1:5, dispersing and mixing uniformly under the blowing of dry air, and settling on a mesh belt to obtain the fiber felt blank.
Wherein the boron nitride precursor fiber is prepared by the following method: boron trichloride and methylamine are used as raw materials, toluene is used as a solvent to prepare a boron nitride precursor, and the boron nitride precursor is heated and melted and then drawn in a constant temperature and humidity environment to obtain the boron nitride.
(2) And carrying out hot pressing treatment on the fiber mat blank to obtain a fiber mat preform.
Specifically, the fiber mat blank is subjected to hot pressing treatment through a hot pressing roller, the pressure is controlled to be 0.01MPa, the temperature is controlled to be 150 ℃, boron nitride precursor fibers in the fiber mat blank are softened, and boron nitride fibers are bonded to form a mat, so that a fiber mat preform is obtained.
(3) And (3) sending the fiber mat preform into a high-temperature furnace to carry out nitriding treatment at 950 ℃ in an ammonia gas and nitrogen gas atmosphere, so that the components of the boron nitride precursor fibers are converted (namely, the boron nitride precursor is converted into boron nitride), and the boron nitride combined boron nitride fiber mat is obtained.
The embodiment also provides the boron nitride fiber mat prepared by the method.
Example 3
The embodiment provides a preparation method of a boron nitride fiber mat, which comprises the following steps:
(1) And (3) chopping, mixing and lapping the boron nitride fibers and the boron nitride precursor fibers to obtain the fiber felt blank.
Specifically, chopping boron nitride fibers into 3-20mm; chopping boron nitride precursor fiber into 3-20mm in a constant temperature and constant humidity environment; adding the chopped boron nitride fibers and boron nitride precursor fibers into a fiber settling chamber according to the weight ratio of 1:1, dispersing and mixing uniformly under the blowing of dry air, and settling on a mesh belt to obtain the fiber felt blank.
Wherein the boron nitride precursor fiber is prepared by the following method: boron trichloride and methylamine are used as raw materials, toluene is used as a solvent to prepare a boron nitride precursor, and the boron nitride precursor is heated and melted and then drawn in a constant temperature and humidity environment to obtain the boron nitride.
(2) And carrying out hot pressing treatment on the fiber mat blank to obtain a fiber mat preform.
Specifically, the fiber mat blank is subjected to hot pressing treatment through a hot pressing roller, the pressure is controlled to be 0.1MPa, the temperature is controlled to be 300 ℃, boron nitride precursor fibers in the fiber mat blank are softened, and boron nitride fibers are bonded to form a mat, so that the fiber mat preform is obtained.
(3) And (3) feeding the fiber felt preform into a high-temperature furnace to carry out nitriding treatment at 1050 ℃ in an ammonia gas and nitrogen gas atmosphere, so that the components of the boron nitride precursor fiber are converted (namely, the boron nitride precursor is converted into boron nitride), and the boron nitride combined boron nitride fiber felt is obtained.
The embodiment also provides the boron nitride fiber mat prepared by the method.
The above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, those skilled in the art may still make modifications to the technical solutions described in the foregoing embodiments, or may make equivalent substitutions for some or all of the technical features thereof; such modifications and substitutions do not depart from the spirit of the invention, and are intended to be included within the scope of the appended claims and description.
Claims (7)
1. The preparation method of the boron nitride fiber mat is characterized by comprising the following steps:
(1) Chopping, mixing and lapping the boron nitride fibers and the boron nitride precursor fibers to obtain a fiber felt blank;
(2) Carrying out hot pressing treatment on the fiber mat blank to obtain a fiber mat preform;
(3) Nitriding the fiber mat preform to obtain a boron nitride fiber mat;
wherein the boron nitride precursor fiber is prepared by the following method: preparing a boron nitride precursor by taking boron trichloride and methylamine as raw materials, heating and melting the boron nitride precursor, and then drawing the wire to obtain the boron nitride precursor;
in the step (1), the boron nitride fiber and the boron nitride precursor fiber are mixed according to the weight ratio of 1:1-5;
in step (1), the boron nitride fibers and boron nitride precursor fibers are chopped into 3-20mm.
2. The preparation method according to claim 1, wherein in step (1), the method specifically comprises the following steps:
chopping boron nitride fibers;
chopping boron nitride precursor fibers;
adding the chopped boron nitride fibers and boron nitride precursor fibers into a fiber settling chamber, dispersing and mixing uniformly under the blowing of dry air, and settling on a mesh belt to obtain the fiber felt blank.
3. The process according to claim 1, wherein in the step (2), the pressure is 0.01 to 0.1MPa and the temperature is 150 to 300 ℃.
4. The method according to claim 1, wherein in the step (2), a heat press roller is used for the heat press treatment.
5. The method according to claim 1, wherein in the step (3), the nitriding treatment is performed at a temperature of 950 to 1050 ℃.
6. The method according to claim 1, wherein in the step (3), the atmosphere is ammonia and nitrogen during the nitriding treatment.
7. A boron nitride fiber mat produced by the production method according to any one of claims 1 to 6.
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| CN202211215367.6A CN115385705B (en) | 2022-09-30 | 2022-09-30 | Boron nitride fiber mat and preparation method thereof |
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| CN202211215367.6A CN115385705B (en) | 2022-09-30 | 2022-09-30 | Boron nitride fiber mat and preparation method thereof |
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| CN115385705B true CN115385705B (en) | 2023-08-18 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2581057A1 (en) * | 1985-04-29 | 1986-10-31 | Elimination Indle Sarl Franc | Fluid composition for the production of protective layers which can be used as a coating or mulching and for the production of panels, and products produced |
| CN105525438A (en) * | 2016-01-20 | 2016-04-27 | 山东工业陶瓷研究设计院有限公司 | Boron nitride fiber mat and preparation method thereof |
| CN106810286A (en) * | 2017-01-19 | 2017-06-09 | 哈尔滨工业大学 | A kind of boron nitride fiber enhancing cordierite ceramic based composites and preparation method thereof |
| JP2020186479A (en) * | 2019-05-10 | 2020-11-19 | トヨタ紡織株式会社 | Method of manufacturing base material, and apparatus of manufacturing base material |
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- 2022-09-30 CN CN202211215367.6A patent/CN115385705B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2581057A1 (en) * | 1985-04-29 | 1986-10-31 | Elimination Indle Sarl Franc | Fluid composition for the production of protective layers which can be used as a coating or mulching and for the production of panels, and products produced |
| CN105525438A (en) * | 2016-01-20 | 2016-04-27 | 山东工业陶瓷研究设计院有限公司 | Boron nitride fiber mat and preparation method thereof |
| CN106810286A (en) * | 2017-01-19 | 2017-06-09 | 哈尔滨工业大学 | A kind of boron nitride fiber enhancing cordierite ceramic based composites and preparation method thereof |
| JP2020186479A (en) * | 2019-05-10 | 2020-11-19 | トヨタ紡織株式会社 | Method of manufacturing base material, and apparatus of manufacturing base material |
Non-Patent Citations (1)
| Title |
|---|
| 有机前驱体法制备氮化硼纤维的研究进展;周莹莹等;《合成纤维》;20130625(第06期);第35-37页 * |
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