CN104844222A - 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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- CN104844222A CN104844222A CN201510204140.5A CN201510204140A CN104844222A CN 104844222 A CN104844222 A CN 104844222A CN 201510204140 A CN201510204140 A CN 201510204140A CN 104844222 A CN104844222 A CN 104844222A
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- boric oxide
- boron nitride
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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, be specifically related to a kind of method utilizing presoma conversion process to prepare boron nitride fibre cloth.
Background technology
The good characteristics such as boron nitride ceramics fibre has high temperature resistant (inert atmosphere 3000 DEG C), resistance to chemical attack, dielectric properties are excellent, electrical insulating property good, thermal conductivity is good.The research of domestic boron nitride ceramics fibre has had the developing history of nearly 40 years, boron nitride ceramics fibre to experienced by the product types such as fixed length boron nitride fibre, continuous nitride boron fibre, boron-nitride fibre composite, boron nitride fibre paper.The Application Areas of boron nitride fibre is also in continuous expansion, utilize the excellent properties of boron nitride fibre, the various matrix material made and product can be applicable to the sophisticated technology fields such as Aeronautics and Astronautics, electric power, electronics, comprise the high-end technical fields such as high temperature wave-transparent material, weapon, military equipment power-supply system, nuclear industry, electric automobile power supply system, heat insulation material.Along with the further investigation of applying in each high-end field boron nitride ceramics fibre, more and more urgent to the demand of boron nitride fiber fabric.
Ceramic fiber cloth is woven on a large scale finished product pottery yarn by the braiding apparatus of mechanize as the preparation technology of the product such as glasscloth, carbon cloth, this processing requirement pottery yarn tensile strength is high, snappiness, folding resistance are good, performance is homogeneous, consistent, and there is the continuous length meeting woven requirement.
The tensile strength of boron nitride ceramics fibre yarn, folding resistance and performance uniformity can not meet the performance requriements of mechanize braiding apparatus to yarn, cannot operate the computer, the thinking therefore adopting mechanised equipment directly to weave boron nitride fibre cloth is impracticable at present.
In sum; need the exploitation of boron nitride fibre cloth that carry out a kind of high comprehensive performance, that be easy to large-scale production badly; solve the demand to basic raw material in high temperature wave-transparent material, heat insulation material preparation process, also solve and prepare problem in the mass-producing of field of power systems barrier film.
Summary of the invention
The object of this invention is to provide a kind of method utilizing presoma conversion process to prepare boron nitride fibre cloth; technique is simple; be easy to accomplish scale production; solve the problem can not directly weaved cotton cloth because of boron nitride fibre undercapacity, the preparation for high temperature wave-transparent material, heat insulation material and battery diaphragm provides the basic raw material of excellent performance.
The method utilizing presoma conversion process to prepare boron nitride fibre cloth of the present invention, comprises the following steps:
(1) boric acid is converted into single bundle boric oxide fibre yarn: by boric acid fusing, wire drawing, obtains single bundle boric oxide fibre yarn;
(2) pool capital and twist with the fingers, weave: 2 ~ 10 bundle boric oxide fibre yarns pool capital and is twisted as and singly restraint boric oxide fibre rove, and boric oxide fibre rove is woven into boric oxide fibre cloth;
(3) low temperature nitride thermal treatment: boric oxide fibre cloth is carried out low temperature nitride thermal treatment under ammonia atmosphere, obtains boron nitride fibre cloth;
(4) high-temperature heat treatment: boron nitride fibre cloth is carried out high-temperature heat treatment.
Wherein, preferred technical scheme is as follows:
The temperature of fusion of step (1) boric acid is 800 ~ 1000 DEG C, and fusing time is 5 ~ 10h.
Step (1) adopts bushing and drawing wire machine cooperation to carry out wire drawing, and bushing temperature is 600 ~ 800 DEG C, and mandrel rotating speed is 3500 ~ 5000 revs/min.
Number of fiber in step (1) single bundle boric oxide fibre yarn is 50 ~ 500, and the diameter of single fiber is 5 ~ 10 μm.
Step (3) low temperature nitride heat treatment process parameter is: ammonia flow is 1 ~ 5m
3/ h, temperature rise rate is 30 ~ 50 DEG C/min, is warming up to 600 ~ 800 DEG C, insulation 2 ~ 5h.Low temperature nitride thermal treatment adopts low temperature nitride stove to carry out.
Step (4) high-temperature heat treatment process parameter is: temperature rise rate is 8 ~ 20 DEG C/h, is warming up to 1400 ~ 1500 DEG C, insulation 1 ~ 3h.High-temperature heat treatment adopts high temperature heat treatment furnace to carry out.
Presoma of the present invention is boron oxide.
Beneficial effect of the present invention is as follows:
(1) the present invention is designed by braiding structure, first adopts weaving braiding boric oxide fibre cloth, then utilizes presoma conversion process, optimize nitriding process parameter, control the temperature rate of critical process point, by boric oxide fibre cloth nitriding treatment, change into boron nitride fibre cloth.
(2) the boron nitride fibre cloth that prepared by the present invention not only has the appearance characteristics of common cloth, smooth, soft, also has that high temperature resistant, resistance to chemical attack, wave transparent, electrical property are excellent, electrolytic solution high adsorption capacity, the overall characteristics such as long lifetime.
(3) the boron nitride fibre cloth that prepared by the present invention can be used as the diaphragm material of high-temperature molten salt battery, fabric is prepared by the technique such as acupuncture, stitching, also as the strongthener of ultrahigh-temperature anti-yaw damper electromagnetic wave transparent material, can also can use as high temperature heat insulation material, high-temperature-resistant filtering material.
(4) preparation technology of the present invention is simple, is easy to accomplish scale production.
Accompanying drawing explanation
Fig. 1 is the boron nitride fibre cloth photo prepared with the present invention.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
By 5kg boric acid in material crucible 800 DEG C fusing 5 hours, until fused solution is transparent, clarification, bubble-free.Carry out wire drawing with 200 hole platinum bushings, nozzle plate temperature is 600 DEG C, and mandrel rotating speed is 3500 revs/min, and to obtain number of fiber be the diameter of 200 is the boric oxide fibre yarn of 8.2 μm.By the boric oxide fibre yarn of 2 of gained bundle 200, utilization is pooled capital and equipment of twisting with the fingers is pooled capital, and obtains the boric oxide fibre rove of 400.
Utilize braiding apparatus to weave boric oxide fibre rove, braiding sample is incubated 2h under 600 DEG C of ammonia atmospheres, and ammonia flow is 1m
3/ h, temperature rise rate are 30 DEG C/min, obtain the boron nitride fibre cloth of low temperature nitride.By above cloth 1400 DEG C of high-temperature heat treatment 60min in vacuum carbon tube furnace, temperature rise rate is 8 DEG C/h, obtains boron nitride fibre cloth.
Prepared boron nitride fibre cloth thickness is 304 μm, and area density is 185g/m
2, tensile strength is 540g/15mm.
Embodiment 2
By 5kg boric acid in material crucible 800 DEG C fusing 5 hours, until fused solution is transparent, clarification, bubble-free.Carry out wire drawing with 200 hole platinum bushings, nozzle plate temperature is 700 DEG C, and mandrel rotating speed is 4000 revs/min, and to obtain number of fiber be the diameter of 200 is the boric oxide fibre yarn of 8.3 μm.By the boric oxide fibre yarn of 5 of gained bundle 200, utilization is pooled capital and equipment of twisting with the fingers is pooled capital, and obtains the boric oxide fibre rove of 1000.
Utilize braiding apparatus to weave boric oxide fibre rove, braiding sample is incubated 4h under 750 DEG C of ammonia atmospheres, and ammonia flow is 3m
3/ h, temperature rise rate are 40 DEG C/min, obtain the boron nitride fibre cloth of low temperature nitride.By above cloth 1450 DEG C of high-temperature heat treatment 80min in vacuum carbon tube furnace, temperature rise rate is 10 DEG C/h, obtains boron nitride fibre cloth.
Prepared boron nitride fibre cloth thickness is 500 μm, and area density is 450g/m
2, tensile strength is 700g/15mm.
Embodiment 3
By 5kg boric acid in material crucible 900 DEG C fusing 10 hours, until fused solution is transparent, clarification, bubble-free.Carry out wire drawing with 200 hole platinum bushings, nozzle plate temperature is 700 DEG C, and mandrel rotating speed is 3800 revs/min, and to obtain number of fiber be the diameter of 200 is the boric oxide fibre yarn of 7 μm.By the boric oxide fibre yarn of 5 of gained bundle 200, utilization is pooled capital and equipment of twisting with the fingers is pooled capital, and obtains the boric oxide fibre rove of 1000.
Utilize braiding apparatus to weave boric oxide fibre rove, braiding sample is incubated 3h under 700 DEG C of ammonia atmospheres, and ammonia flow is 4m
3/ h, temperature rise rate are 45 DEG C/min, obtain the boron nitride fibre cloth of low temperature nitride.By above cloth in vacuum carbon tube furnace under 1480 DEG C of nitrogen atmospheres, high-temperature heat treatment 60min, temperature rise rate is 10 DEG C/h, obtains boron nitride fibre cloth.
Prepared boron nitride fibre cloth thickness is 450 μm, and area density is 380g/m
2, tensile strength is 750g/15mm.
Embodiment 4
By 5kg boric acid in material crucible 1000 DEG C fusing 10 hours, until fused solution is transparent, clarification, bubble-free.Carry out wire drawing with 200 hole platinum bushings, nozzle plate temperature is 800 DEG C, and mandrel rotating speed is 5000 revs/min, and to obtain number of fiber be the diameter of 200 is the boric oxide fibre yarn of 6.9 μm.By the boric oxide fibre yarn of 10 of gained bundle 200, utilization is pooled capital and equipment of twisting with the fingers is pooled capital, and obtains the boric oxide fibre rove of 2000.
Utilize braiding apparatus to weave boric oxide fibre rove, braiding sample is incubated 5h under 800 DEG C of ammonia atmospheres, and ammonia flow is 5m
3/ h, temperature rise rate are 50 DEG C/min, obtain the boron nitride fibre cloth of low temperature nitride.By above cloth 1500 DEG C of high-temperature heat treatment 180min in vacuum carbon tube furnace, temperature rise rate is 20 DEG C/h, obtains boron nitride fibre cloth.
Prepared boron nitride fibre cloth thickness is 440 μm, and area density is 375g/m
2, tensile strength is 690g/15mm.
Claims (6)
1. utilize presoma conversion process to prepare a method for boron nitride fibre cloth, it is characterized in that comprising the following steps:
(1) boric acid is converted into single bundle boric oxide fibre yarn: by boric acid fusing, wire drawing, obtains single bundle boric oxide fibre yarn;
(2) pool capital and twist with the fingers, weave: 2 ~ 10 bundle boric oxide fibre yarns pool capital and is twisted as and singly restraint boric oxide fibre rove, and boric oxide fibre rove is woven into boric oxide fibre cloth;
(3) low temperature nitride thermal treatment: boric oxide fibre cloth is carried out low temperature nitride thermal treatment under ammonia atmosphere, obtains boron nitride fibre cloth;
(4) high-temperature heat treatment: boron nitride fibre cloth is carried out high-temperature heat treatment.
2. the method utilizing presoma conversion process to prepare boron nitride fibre cloth according to claim 1, is characterized in that: the temperature of fusion of step (1) boric acid is 800 ~ 1000 DEG C, and fusing time is 5 ~ 10h.
3. the method utilizing presoma conversion process to prepare boron nitride fibre cloth according to claim 1, it is characterized in that: step (1) adopts bushing and drawing wire machine cooperation to carry out wire drawing, bushing temperature is 600 ~ 800 DEG C, and mandrel rotating speed is 3500 ~ 5000 revs/min.
4. the method utilizing presoma conversion process to prepare boron nitride fibre cloth according to claim 1, is characterized in that: the number of fiber in step (1) single bundle boric oxide fibre yarn is 50 ~ 500, and the diameter of single fiber is 5 ~ 10 μm.
5. the method utilizing presoma conversion process to prepare boron nitride fibre cloth according to claim 1, is characterized in that: step (3) low temperature nitride heat treatment process parameter is: ammonia flow is 1 ~ 5m
3/ h, temperature rise rate is 30 ~ 50 DEG C/min, is warming up to 600 ~ 800 DEG C, insulation 2 ~ 5h.
6. the method utilizing presoma conversion process to prepare boron nitride fibre cloth according to claim 1, it is characterized in that: step (4) high-temperature heat treatment process parameter is: temperature rise rate is 8 ~ 20 DEG C/h, be warming up to 1400 ~ 1500 DEG C, insulation 1 ~ 3h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107540382A (en) * | 2017-08-18 | 2018-01-05 | 山东工业陶瓷研究设计院有限公司 | A kind of boron nitride continuous fiber and its preparation technology and application |
| CN107557907A (en) * | 2017-08-18 | 2018-01-09 | 山东工业陶瓷研究设计院有限公司 | A kind of boron nitride chopped fiber and its preparation technology and application |
| CN115611635A (en) * | 2022-12-14 | 2023-01-17 | 山东工业陶瓷研究设计院有限公司 | Boron nitride fiber and preparation method and application thereof |
| CN115626829A (en) * | 2022-12-07 | 2023-01-20 | 山东工业陶瓷研究设计院有限公司 | Boron nitride fiber and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107540382A (en) * | 2017-08-18 | 2018-01-05 | 山东工业陶瓷研究设计院有限公司 | A kind of boron nitride continuous fiber and its preparation technology and application |
| CN107557907A (en) * | 2017-08-18 | 2018-01-09 | 山东工业陶瓷研究设计院有限公司 | A kind of boron nitride chopped fiber and its preparation technology and application |
| 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 |
| CN115626829A (en) * | 2022-12-07 | 2023-01-20 | 山东工业陶瓷研究设计院有限公司 | Boron nitride fiber and preparation method thereof |
| CN115611635A (en) * | 2022-12-14 | 2023-01-17 | 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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