CN104844222B - Method for preparing boron nitride fiber cloth by using precursor conversion - Google Patents
Method for preparing boron nitride fiber cloth by using precursor conversion Download PDFInfo
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- CN104844222B CN104844222B CN201510204140.5A CN201510204140A CN104844222B CN 104844222 B CN104844222 B CN 104844222B CN 201510204140 A CN201510204140 A CN 201510204140A CN 104844222 B CN104844222 B CN 104844222B
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- boric oxide
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Abstract
The invention specifically relates to a method for preparing boron nitride fiber cloth by using precursor conversion, which belongs to the technical field of ceramic materials. The method comprises the following steps: (1) subjecting boric acid to fusing and wire drawing so as to obtain single-bunch boric oxide fiber yarns; (2) stranding and cabling 2 to 10 boric oxide fiber yarns into a thick single-bunch boric oxide fiber yarn and braiding the thick single-bunch boric oxide fiber yarn to obtain boric oxide fiber cloth; (3) subjecting the boric oxide fiber cloth to low-temperature nitridation heat treatment in an ammonia gas atmosphere so as to obtain boric oxide fiber cloth; and (4) carrying out high-temperature heat treatment on the boric oxide fiber cloth. The method provided by the invention is simple, can easily realize large-scale production, overcomes the problem of incapable direct weaving due to insufficient strength of boron nitride fiber, and provides a basic raw material with excellent performance for preparation of high-temperature wave-transmitting materials, heatproof materials and battery diaphragms.
Description
Technical field
The invention belongs to technical field of ceramic material, and in particular to a kind of to prepare boron nitride fibre using presoma conversion process
The method of dimension cloth.
Background technology
Boron nitride ceramics fibre has high temperature resistant (3000 DEG C of inert atmosphere), resistance to chemical attack, dielectric properties excellent, electric exhausted
The good characteristic such as edge is good, heat conductivity is good.The research of domestic boron nitride ceramics fibre has had the developing history of nearly 40 years, nitridation
Boron ceramic fibre experienced fixed length boron nitride fiber, continuous nitride boron fibre, boron-nitride fibre composite, boron nitride fiber paper
Etc. product type.The application of boron nitride fiber is also constantly extending, and using the excellent properties of boron nitride fiber, that what is made is each
Plant composite and product can be applicable to the sophisticated technology such as Aeronautics and Astronautics, electric power, electronics field, including high temperature wave-transparent material, force
The high-end technical fields such as device, military equipment power-supply system, nuclear industry, electric automobile power supply system, heat insulation material.With to nitridation
Further investigation of the boron ceramic fibre in each high-end field application, it is more and more urgent to the demand of boron nitride fiber fabric.
Braiding of the preparation technology of the ceramic fiber cloth such as product such as glass fabric, carbon cloth generally by mechanization
Equipment is woven on a large scale to finished product ceramics yarn, this technological requirement ceramics yarn tensile strength height, pliability, folding resistance
Good, performance is homogeneous, consistent, and with meeting the continuous length of woven requirement.
The tensile strength of boron nitride ceramics fibre yarn, folding resistance and performance uniformity can not meet mechanization braiding apparatus
Performance requirement to yarn, it is impossible to operate the computer, therefore the thinking mesh of boron nitride fiber cloth is directly woven using mechanized equipment
Before be impracticable.
In sum, need a kind of opening for boron nitride fiber cloth carrying out high comprehensive performance, being easy to large-scale production badly
Send out, the demand in solution high temperature wave-transparent material, heat insulation material preparation process to basic raw material is also solved in field of power systems
Barrier film prepare with scale problem.
The content of the invention
It is an object of the invention to provide a kind of method that utilization presoma conversion process prepares boron nitride fiber cloth, technique letter
It is single, it is easy to accomplish large-scale production, solve the problems, such as directly to weave cotton cloth because of boron nitride fiber intensity deficiency, be high temperature wave transparent
Basic raw material of the preparation of material, heat insulation material and battery diaphragm there is provided excellent performance.
The method that utilization presoma conversion process of the present invention prepares boron nitride fiber cloth, comprises the following steps：
(1) boric acid is converted into single beam boric oxide fibre yarn：By boric acid fusing, wire drawing, single beam boric oxide fibre yarn is obtained
Line；
(2) pool capital and twist with the fingers, weave：2～10 beam boric oxide fibre yarns are pooled capital and single beam boric oxide fibre rove is twisted as,
And boric oxide fibre rove is woven into into boric oxide fibre cloth；
(3) low temperature nitride heat treatment：Boric oxide fibre cloth is carried out into low temperature nitride heat treatment under ammonia atmosphere, nitrogen is obtained
Change boron fibre cloth；
(4) high-temperature heat treatment：Boron nitride fiber cloth is carried out into high-temperature heat treatment.
Wherein, preferred technical scheme is as follows：
The fusion temperature of step (1) boric acid is 800～1000 DEG C, and fusing time is 5～10h.
Step (1) is coordinated using bushing and wire drawing machine carries out wire drawing, and bushing temperature is 600～800 DEG C, wire drawing
Head rotating speed is 3500～5000 revs/min.
Number of fiber in step (1) list beam boric oxide fibre yarn is 50～500, single fiber a diameter of 5～
10μm。
Step (3) low temperature nitride heat treatment process parameter is：Ammonia flow is 1～5m3/ h, heating rate are 30～50
DEG C/min, 600～800 DEG C are warming up to, 2～5h is incubated.Low temperature nitride heat treatment is carried out using low temperature nitride stove.
Step (4) high-temperature heat treatment process parameter is：Heating rate is 8～20 DEG C/h, is warming up to 1400～1500 DEG C, is protected
1～3h of temperature.High-temperature heat treatment is carried out using high temperature heat treatment furnace.
Presoma of the present invention is boron oxide.
Beneficial effects of the present invention are as follows：
(1) present invention is designed by braiding structure, first weaves boric oxide fibre cloth using weaving, then using forerunner
Body conversion process, optimizes nitriding process parameter, controls the temperature rate of critical process point, at boric oxide fibre cloth nitridation
Reason, changes into boron nitride fiber cloth.
(2) boron nitride fiber cloth prepared by the present invention not only has the appearance characteristics of common cloth, smooth, soft, also has
The overall characteristics such as high temperature resistant, resistance to chemical attack, wave transparent, excellent electrical properties, electrolyte high adsorption capacity, long-life.
(3) boron nitride fiber cloth prepared by the present invention can serve as the diaphragm material of high-temperature molten salt battery, by acupuncture, seam
The techniques such as conjunction prepare fabric, it is also possible to as the reinforcing material of superhigh temperature anti-yaw damper electromagnetic wave transparent material, be also used as high temperature solar heat protection
Material, high-temperature-resistant filtering material are used.
(4) preparation process is simple of the present invention, it is easy to accomplish large-scale production.
Description of the drawings
Fig. 1 is the boron nitride fiber cloth photo prepared with the present invention.
Specific embodiment
With reference to embodiments the present invention is described further.
Embodiment 1
5kg boric acid is melted 5 hours for 800 DEG C in the material crucible, until fused solution is transparent, clarification, till bubble-free.With
200 hole platinum bushings carry out wire drawing, and nozzle plate temperature is 600 DEG C, and mandrel rotating speed is 3500 revs/min, obtains fibrous root
Number is the boric oxide fibre yarn of a diameter of 8.2 μm of 200.By the boric oxide fibre yarn of 2 beam 200 of gained, utilize
Pool capital and twist with the fingers equipment to be pooled capital, obtain the boric oxide fibre rove of 400.
Boric oxide fibre rove is woven using braiding apparatus, braiding sample is incubated 2h under 600 DEG C of ammonia atmospheres,
Ammonia flow is 1m3/ h, heating rate are 30 DEG C/min, obtain the boron nitride fiber cloth of low temperature nitride.Above fiber cloth is existed
1400 DEG C of high-temperature heat treatments 60min in vacuum carbon tube furnace, heating rate are 8 DEG C/h, obtain boron nitride fiber cloth.
Prepared boron nitride fiber cloth thickness is 304 μm, and surface density is 185g/m2, tensile strength is 540g/15mm.
Embodiment 2
5kg boric acid is melted 5 hours for 800 DEG C in the material crucible, until fused solution is transparent, clarification, till bubble-free.With
200 hole platinum bushings carry out wire drawing, and nozzle plate temperature is 700 DEG C, and mandrel rotating speed is 4000 revs/min, obtains fibrous root
Number is the boric oxide fibre yarn of a diameter of 8.3 μm of 200.By the boric oxide fibre yarn of 5 beam 200 of gained, utilize
Pool capital and twist with the fingers equipment to be pooled capital, obtain the boric oxide fibre rove of 1000.
Boric oxide fibre rove is woven using braiding apparatus, braiding sample is incubated 4h under 750 DEG C of ammonia atmospheres,
Ammonia flow is 3m3/ h, heating rate are 40 DEG C/min, obtain the boron nitride fiber cloth of low temperature nitride.Above fiber cloth is existed
1450 DEG C of high-temperature heat treatments 80min in vacuum carbon tube furnace, heating rate are 10 DEG C/h, obtain boron nitride fiber cloth.
Prepared boron nitride fiber cloth thickness is 500 μm, and surface density is 450g/m2, tensile strength is 700g/15mm.
Embodiment 3
5kg boric acid is melted 10 hours for 900 DEG C in the material crucible, until fused solution is transparent, clarification, till bubble-free.
Wire drawing is carried out with 200 hole platinum bushings, nozzle plate temperature is 700 DEG C, and mandrel rotating speed is 3800 revs/min, obtains fiber
Radical is the boric oxide fibre yarn of a diameter of 7 μm of 200.By the boric oxide fibre yarn of 5 beam 200 of gained, utilize
Pool capital and twist with the fingers equipment to be pooled capital, obtain the boric oxide fibre rove of 1000.
Boric oxide fibre rove is woven using braiding apparatus, braiding sample is incubated 3h under 700 DEG C of ammonia atmospheres,
Ammonia flow is 4m3/ h, heating rate are 45 DEG C/min, obtain the boron nitride fiber cloth of low temperature nitride.Above fiber cloth is existed
In vacuum carbon tube furnace under 1480 DEG C of nitrogen atmospheres, high-temperature heat treatment 60min, heating rate are 10 DEG C/h, obtain boron nitride fiber
Cloth.
Prepared boron nitride fiber cloth thickness is 450 μm, and surface density is 380g/m2, tensile strength is 750g/15mm.
Embodiment 4
5kg boric acid is melted 10 hours for 1000 DEG C in the material crucible, until fused solution is transparent, clarification, till bubble-free.
Wire drawing is carried out with 200 hole platinum bushings, nozzle plate temperature is 800 DEG C, and mandrel rotating speed is 5000 revs/min, obtains fiber
Radical is the boric oxide fibre yarn of a diameter of 6.9 μm of 200.By the boric oxide fibre yarn of 10 beam 200 of gained, profit
Pooled capital with pooling capital and twisting with the fingers equipment, obtained the boric oxide fibre rove of 2000.
Boric oxide fibre rove is woven using braiding apparatus, braiding sample is incubated 5h under 800 DEG C of ammonia atmospheres,
Ammonia flow is 5m3/ h, heating rate are 50 DEG C/min, obtain the boron nitride fiber cloth of low temperature nitride.Above fiber cloth is existed
1500 DEG C of high-temperature heat treatments 180min in vacuum carbon tube furnace, heating rate are 20 DEG C/h, obtain boron nitride fiber cloth.
Prepared boron nitride fiber cloth thickness is 440 μm, and surface density is 375g/m2, tensile strength is 690g/15mm.
Claims (6)
1. a kind of method that utilization presoma conversion process prepares boron nitride fiber cloth, it is characterised in that comprise the following steps：
（1）Boric acid is converted into single beam boric oxide fibre yarn：By boric acid fusing, wire drawing, single beam boric oxide fibre yarn is obtained；
（2）Pool capital and twist with the fingers, weave：2～10 beam boric oxide fibre yarns are pooled capital and single beam boric oxide fibre rove is twisted as, and will
Boric oxide fibre rove is woven into boric oxide fibre cloth；
（3）Low temperature nitride heat treatment：By boric oxide fibre cloth under ammonia atmosphere, carry out at low temperature nitride heat in 600～800 DEG C
Reason, obtains boron nitride fiber cloth；
（4）High-temperature heat treatment：Boron nitride fiber cloth is carried out into high-temperature heat treatment.
2. the method that utilization presoma conversion process according to claim 1 prepares boron nitride fiber cloth, it is characterised in that：
Step（1）The fusion temperature of boric acid is 800～1000 DEG C, and fusing time is 5～10h.
3. the method that utilization presoma conversion process according to claim 1 prepares boron nitride fiber cloth, it is characterised in that：
Step（1）Being coordinated using bushing and wire drawing machine carries out wire drawing, and bushing temperature is 600～800 DEG C, mandrel
Rotating speed is 3500～5000 revs/min.
4. the method that utilization presoma conversion process according to claim 1 prepares boron nitride fiber cloth, it is characterised in that：
Step（1）Number of fiber in single beam boric oxide fibre yarn is 50～500, a diameter of 5～10 μm of single fiber.
5. the method that utilization presoma conversion process according to claim 1 prepares boron nitride fiber cloth, it is characterised in that：
Step（3）Low temperature nitride heat treatment process parameter is：Ammonia flow is 1～5m3/ h, heating rate are 30～50 DEG C/min, are risen
Temperature is incubated 2～5h to 600～800 DEG C.
6. the method that utilization presoma conversion process according to claim 1 prepares boron nitride fiber cloth, it is characterised in that：
Step（4）High-temperature heat treatment process parameter is：Heating rate is 8～20 DEG C/h, is warming up to 1400～1500 DEG C, insulation 1
～3h.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105977431A (en) * | 2016-06-23 | 2016-09-28 | 山东工业陶瓷研究设计院有限公司 | Preparation method for boron nitride fiber diaphragm for lithium-system thermal battery |
| CN107540382B (en) * | 2017-08-18 | 2020-05-19 | 山东工业陶瓷研究设计院有限公司 | Boron nitride continuous fiber and preparation process and application thereof |
| CN107557907B (en) * | 2017-08-18 | 2020-06-23 | 山东工业陶瓷研究设计院有限公司 | Boron nitride short fiber and preparation process and application thereof |
| CN115626829B (en) * | 2022-12-07 | 2023-03-21 | 山东工业陶瓷研究设计院有限公司 | Boron nitride fiber and preparation method thereof |
| CN115611635B (en) * | 2022-12-14 | 2023-03-21 | 山东工业陶瓷研究设计院有限公司 | Boron nitride fiber and preparation method and application thereof |
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| CN101254904A (en) * | 2008-02-22 | 2008-09-03 | 哈尔滨工业大学深圳研究生院 | Method for preparing boron nitride continuous nano fibre |
| CN101428813A (en) * | 2008-12-17 | 2009-05-13 | 哈尔滨工业大学深圳研究生院 | Process for producing ultra-fine boron nitride continuous nano-fibre |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101254904A (en) * | 2008-02-22 | 2008-09-03 | 哈尔滨工业大学深圳研究生院 | Method for preparing boron nitride continuous nano fibre |
| CN101428813A (en) * | 2008-12-17 | 2009-05-13 | 哈尔滨工业大学深圳研究生院 | Process for producing ultra-fine boron nitride continuous nano-fibre |
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