CN117602951A - A continuous preparation method of BN coating on SiC fiber surface - Google Patents
A continuous preparation method of BN coating on SiC fiber surface Download PDFInfo
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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Abstract
本发明公开了一种连续制备SiC纤维表面BN涂层的方法，先于SiC纤维表面预先设置碳涂层，然后再置于连续化的设备中，将SiC纤维由放丝装置中放出，先浸润在含硼的溶液中获得被含硼薄膜包裹的SiC纤维，然后将被含硼薄膜包裹的SiC纤维继续经过高温炉于SiC纤维表面形成BN涂层，所述高温炉中通入氮气和氨气的混合气氛；再经收丝装置收丝，本发明在SiC纤维上制备BN涂层的温度高，涂层结晶性好，稳定性高，在复合材料的制备过程中可有效保护纤维。
The invention discloses a method for continuously preparing the BN coating on the surface of SiC fiber. The carbon coating is pre-set on the surface of the SiC fiber, and then placed in a continuous equipment. The SiC fiber is released from the wire releasing device and first soaked. The SiC fiber wrapped with the boron-containing film is obtained in a boron-containing solution, and then the SiC fiber wrapped with the boron-containing film continues to pass through a high-temperature furnace to form a BN coating on the surface of the SiC fiber. Nitrogen and ammonia gas are passed into the high-temperature furnace. The mixed atmosphere; and then the yarn is collected by the yarn collecting device. The method of the present invention prepares the BN coating on the SiC fiber at a high temperature. The coating has good crystallinity and high stability, and can effectively protect the fiber during the preparation process of the composite material.
Description
Technical Field
The invention belongs to the field of preparation of fiber surface interface layers, and particularly relates to a method for continuously preparing a SiC fiber bundle surface BN coating.
Background
The SiC fiber reinforced ceramic matrix composite has the excellent characteristics of high temperature resistance, oxidation resistance, corrosion resistance, light weight and high strength, and has a very large application prospect in the field of aerospace and military industry. The fiber interface coating has the important functions of protecting fibers and regulating the binding force between the fibers and the matrix, and is a key for preparing the composite material with excellent performance.
BN coating as an interface coating for SiC fibers has the following advantages: 1. the BN coating is the same as the C coating, is weak interface bonding, can better exert the bearing capacity of the brittle SiC fiber, and improves the strength and fracture toughness of the SiC fiber reinforced ceramic matrix composite; 2. the BN coating has excellent antioxidation capability, and B generated after BN oxidation 2 O 3 Has self-healing function and can prevent further oxidation. 3. The BN coating has strong corrosion resistance and can well protect fibers in the preparation process of the composite material.
At present, the conventional method for preparing BN interface layer on the surface of SiC fiber comprises the following steps: siC fibers are first woven into shape and then deposited in a closed deposition furnace. However, since the woven body has a certain thickness, the deposition speeds of the outer layer and the inner layer are different, the uniformity of the coating is greatly different, and the situation that the surface coating layer is thick and the core coating layer is thin is easy to occur. In addition, the temperature for preparing the BN coating by chemical vapor deposition is lower, is in an amorphous state and is easy to decompose, the amorphous BN needs to be further subjected to high-temperature heat treatment in other equipment to be converted into crystalline BN, and the coating is easy to decompose in the transfer process, so that the high-crystalline BN coating is not beneficial to being obtained.
Zhou Xingui et al used dip coating to impregnate SiC fibers in boric acid, urea solution and pyrolysed under ammonia gas for multiple cycles to prepare BN coatings on SiC fiber surfaces, but the preparation temperature was only 1000 ℃, the prepared BN coatings were poor in crystallinity and had the potential for corrosion of the fibers. The Malus asiatica et al adopt a chemical vapor deposition method to continuously deposit a BN coating on SiC fibers, and assisted by high-temperature heat treatment, so that the continuous BN coating with good crystallinity is obtained, but the requirements on equipment are high, the corrosiveness of byproducts is high, and the equipment is extremely easy to damage.
The BN coating with low cost, high production efficiency and good uniformity and stability is developed and obtained, and the process preparation method is further required to be further expanded.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for continuously preparing the BN coating on the surface of the SiC fiber bundle, the preparation method is simple and efficient, the prepared BN interface layer can be uniformly distributed on the surface of the SiC fiber, the fiber is prepared under tension, the flatness of the obtained SiC fiber bundle with the BN coating is good, the braiding property is strong, and the method can be used for preparing high-performance ceramic matrix composite materials.
In order to achieve the above object, the technical scheme of the present invention is as follows:
the invention relates to a method for continuously preparing a BN coating on the surface of a SiC fiber, which comprises the steps of presetting a carbon coating on the surface of the SiC fiber, then placing the SiC fiber in continuous equipment, discharging the SiC fiber from a wire discharging device, firstly soaking the SiC fiber in a boron-containing solution to obtain the SiC fiber wrapped by a boron-containing film, continuously passing the SiC fiber wrapped by the boron-containing film through a high-temperature furnace to form the BN coating on the surface of the SiC fiber, and then collecting wires by a wire collecting device;
introducing a mixed atmosphere of nitrogen and ammonia into the high-temperature furnace;
the boron-containing solution comprises the following components in percentage by mass: 2-10% of boron oxide and 85-96% of absolute ethyl alcohol; PVB 0.5-5%.
According to the invention, siC fibers provided with a carbon coating are discharged from a wire discharge device in continuous equipment, are firstly moved into a boron-containing solution, are soaked in the boron-containing solution to obtain SiC fibers wrapped by a boron-containing film, and then continuously pass through a high-temperature tube furnace, a mixed atmosphere of nitrogen and ammonia is introduced into the high-temperature tube furnace, so that the SiC fibers take the carbon coating as a reaction substrate, and the carbon reacts with boron oxide in the boron-containing film under an ammonia environment to generate BN (boron nitride) to obtain the SiC fiber surface BN coating.
The inventors found that it is ultimately important to be able to obtain a uniform BN coating, that the formulation of the boron-containing solution used, either in place of the ingredients or in any case outside the scope of the present invention, will not result in a uniform BN coating, that during the actual discovery process, the present invention also contemplates other sources of boron, such as boric acid, which not only corrode the fibers but also cause damage to the furnace, and that, in terms of the amount of ingredients, if the PVB is added too much, the boron-containing material applied to the fibers is not sufficiently uniform, affecting the uniformity of the coating, the PVB is added too little, the boron-containing material adhering to the fibers will be reduced, and the thickness of the coating will be too thin;
in addition, the formation of the carbon coating is also important, the carbon coating is not arranged, and the BN coating is directly made at the back of the carbon coating, so that the strength is reduced due to corrosion of the fiber.
Preferably, the SiC fibers comprise monofilament SiC fibers and SiC fiber bundles.
In a preferred scheme, the mode of presetting the carbon coating on the surface of the SiC fiber is as follows: placing the SiC fibers in a heating furnace, introducing a chlorine atmosphere, and preserving the temperature for 1-5 h at 500-800 ℃ to obtain the SiC fiber. In the actual operation process, after adding SiC fibers into a heating furnace, firstly filling inert gas, vacuumizing, repeating for three times, then filling chlorine, keeping the pressure in the furnace in a micro-positive pressure state, then heating to a heat preservation temperature, and preparing a thin carbon coating growing in situ on the surface of the SiC fibers.
The setting method of the carbon coating of the invention etches Si in SiC at high temperature under chlorine atmosphere to become SiCl 4 The gas runs off, and C in the SiC is left to form a carbon coating on the surface, and the carbon coating grown in situ by the method has extremely high bonding performance and extremely good uniformity.
In the actual search, the inventors tried chemical vapor deposition of pyrolytic carbon interfacial layers, and found that not only the bonding performance was reduced, but also the uniformity was far inferior to the present invention.
Preferably, the boron-containing solution comprises the following components in percentage by mass: 3-9% of boron oxide and 90-96% of absolute ethyl alcohol; PVB 1-2%.
In a preferred scheme, the running speed of the SiC fibers is 0.3-3 m/min, and preferably 0.5-2 m/min.
In the invention, the running speed of the SiC fibers or the SiC fiber bundles refers to the linear speed generated by the single SiC fibers or the SiC fiber bundles in motion under the guidance of a wire unwinding device. The wire running speed is controlled within the range of the invention, so that a uniform BN coating can be efficiently obtained.
In a preferred scheme, the flow volume ratio of the nitrogen to the ammonia is 0.8-3:0.5-5. The flow volume ratio of the nitrogen to the ammonia is controlled within the range, so that the efficiency is highest.
Preferably, the temperature of the high-temperature furnace is 1200-1500 ℃.
In a preferred embodiment, the BN coating is 100-800 nm thick and 5-50 nm grain size.
In the preferred scheme, after the BN coating is formed on the surface of the SiC fiber, the SiC fiber is subjected to absolute ethyl alcohol and then is subjected to filament collection through a filament collection device.
Preferably, the continuous equipment comprises a wire unwinding device, a container A, a high-temperature furnace, a container B and a wire winding device; the container A and the container B are positioned at two sides of the high-temperature furnace and communicated with the high-temperature furnace; the container A is filled with boron-containing solution, and the container B is filled with absolute ethyl alcohol.
The invention has the beneficial effects that:
1. the BN coating prepared on the SiC fiber is uniform and controllable in thickness, and the obtained SiC fiber bundle is good in flatness and strong in braiding property, and the performance and uniformity of the ceramic matrix composite material can be greatly improved.
2. The method for preparing the BN coating on the SiC fiber has high temperature, good coating crystallinity and high stability, and can effectively protect the fiber in the preparation process of the composite material.
3. The invention has the advantages of simple equipment, low raw material cost and high efficiency.
Drawings
FIG. 1 is a schematic view of an apparatus for producing BN coating according to the invention.
1 wire feeding device, 2 boron-containing solution (arranged in a container A), 3 process gas inlet, 4 high-temperature tube furnace, 5 tail gas outlet, 6 absolute ethanol solution (arranged in a container B) and 7 wire collecting device.
FIG. 2 is an SEM microstructure of a BN coating prepared according to the invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to better demonstrate the objects, technical solutions and advantages of the present invention. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The preparation in the embodiment is carried out in continuous equipment, wherein the continuous equipment comprises a wire unwinding device, a container A, a high-temperature furnace, a container B and a wire winding device; the container A and the container B are positioned at two sides of the high-temperature furnace and communicated with the high-temperature furnace; the container A is filled with boron-containing solution, and the container B is filled with absolute ethyl alcohol.
The SiC fiber provided with the carbon coating is discharged from the wire unwinding device, firstly moves into the container A, is soaked in the boron-containing solution of the container A, then continuously moves through the high-temperature tube furnace, enters the container B, is soaked in absolute ethyl alcohol, and finally is wound by the wire winding device.
Example 1
Firstly, placing SiC fibers in a heating furnace, filling inert gas, vacuumizing, and repeating for three times. And then introducing chlorine gas, and keeping the pressure in the furnace in a micro-positive pressure state. And then heating to 550 ℃ and preserving heat for 2 hours, and preparing a thin in-situ grown carbon coating on the surface of the SiC fiber.
Boron oxide, absolute ethyl alcohol and PVB are uniformly mixed according to the proportion of 3:96:1 to prepare boron-containing solution. SiC is discharged from a wire unwinding device and is immersed into the prepared boron-containing solution, the wire is conveyed at a speed of 2m/min to pass through a high-temperature tube furnace, the temperature of the high-temperature tube furnace is set to 1400 ℃, the flow ratio of nitrogen to ammonia is 1:1, finally, siC fiber bundles of the BN coating are wound by a wire winding device, the thickness of the coating is 200nm, and the grain size is 7nm.
Example 2
Firstly, placing SiC fibers in a heating furnace, filling inert gas, vacuumizing, and repeating for three times. And then introducing chlorine gas, and keeping the pressure in the furnace in a micro-positive pressure state. And then heating to 650 ℃ and preserving heat for 3 hours, and preparing a thin in-situ grown carbon coating on the surface of the SiC fiber.
Boron oxide and absolute ethyl alcohol are uniformly mixed according to the proportion of 5:93.5:1.5 to prepare boron-containing solution. SiC is discharged from a wire unwinding device and is immersed into the prepared boron-containing solution, the wire is conveyed at a speed of 1.2m/min to pass through a high-temperature tube furnace, the temperature of the high-temperature tube furnace is set to 1450 ℃, the flow ratio of nitrogen to ammonia is 1:2, finally, siC fiber bundles of a BN coating are wound by a wire winding device, the thickness of the coating is 400nm, and the grain size is 10nm.
Example 3
Firstly, placing SiC fibers in a heating furnace, filling inert gas, vacuumizing, and repeating for three times. And then introducing chlorine gas, and keeping the pressure in the furnace in a micro-positive pressure state. And then heating to 750 ℃ and preserving heat for 4 hours, and preparing a thin in-situ grown carbon coating on the surface of the SiC fiber.
Boron oxide, absolute ethyl alcohol and PVB are uniformly mixed according to the proportion of 8:90:2 to prepare boron-containing solution. SiC is discharged from a wire unwinding device and immersed in the prepared boron-containing solution, the wire is conveyed at a speed of 0.6m/min to pass through a high-temperature tube furnace, the temperature of the high-temperature tube furnace is set to 1500 ℃, the flow ratio of nitrogen to ammonia is 1:3, finally SiC fiber bundles of the BN coating are wound by a wire winding device, the thickness of the coating is 700nm, and the grain size is 35nm.
Example 4
Firstly, placing SiC fibers in a heating furnace, filling inert gas, vacuumizing, and repeating for three times. And then introducing chlorine gas, and keeping the pressure in the furnace in a micro-positive pressure state. Then heating to 600 ℃ and preserving heat for 3 hours, and preparing a thin in-situ grown carbon coating on the surface of the SiC fiber.
Boron oxide, absolute ethyl alcohol and PVB are uniformly mixed according to the proportion of 6:92:2 to prepare boron-containing solution. SiC is discharged from a wire unwinding device and is immersed into the prepared boron-containing solution, the wire is conveyed at the speed of 0.8m/min to pass through a high-temperature tube furnace, the temperature of the high-temperature tube furnace is set to 1400 ℃, the flow ratio of nitrogen to ammonia is 1:3, finally, siC fiber bundles of a ribbon BN coating are wound by a wire winding device, the thickness of the coating is 550nm, and the grain size is 27nm.
Example 5
Firstly, placing SiC fibers in a heating furnace, filling inert gas, vacuumizing, and repeating for three times. And then introducing chlorine gas, and keeping the pressure in the furnace in a micro-positive pressure state. And then heating to 700 ℃ and preserving heat for 5 hours, and preparing a thin in-situ grown carbon coating on the surface of the SiC fiber.
Boron oxide, absolute ethyl alcohol and PVB are uniformly mixed according to the proportion of 7:91:2 to prepare boron-containing solution. The SiC is discharged from the wire-releasing device, immersed in the prepared boron-containing solution, and passed through a high-temperature tube furnace at a speed of 0.5m/min, the temperature of the high-temperature tube furnace is set to 1450 ℃, the flow ratio of nitrogen to ammonia is 1:3.5, and finally the SiC fiber bundles of the BN coating are wound by a wire winding device, wherein the thickness of the coating is 600nm, and the grain size is 21nm.
Comparative example 1
Other conditions were the same as in example 1, except that boric oxide was replaced with boric acid of equal weight, and it was found that the BN coating was reduced to about 80nm in thickness and the fiber strength was impaired.
Comparative example 2
Otherwise, the ratio of PVB was reduced and boron oxide, absolute ethyl alcohol and PVB were mixed uniformly in a ratio of 3:96.7:0.3 under the same conditions as in example 1, the viscosity of the resulting boron-containing solution was too low to adhere sufficient boron-containing material to the fibers, and the BN coating was reduced to a thickness of 50nm.
Comparative example 3
Otherwise, the ammonia gas ratio was reduced, the nitrogen gas to ammonia gas flow ratio was changed to 1:0.1, and the BN coating thickness was reduced to 70nm.
Comparative example 4
Otherwise, the wire running speed was increased to 5m/min, the BN coating thickness was reduced to 60nm, and the grain size was reduced to 2nm under the same conditions as in example 1.
Claims (9)
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Citations (6)
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|---|---|---|---|---|
| US6040008A (en) * | 1997-08-04 | 2000-03-21 | University Of Florida | Silicon carbide fibers with boron nitride coatings |
| CN108385087A (en) * | 2018-02-12 | 2018-08-10 | 中南大学 | A method of it is continuous, quick to prepare SiC fiber surface BN coatings |
| CN109553430A (en) * | 2019-01-16 | 2019-04-02 | 苏州宏久航空防热材料科技有限公司 | A kind of SiC with compound interfacef/ SiC ceramic based composites and preparation method thereof |
| CN112624766A (en) * | 2020-12-29 | 2021-04-09 | 哈尔滨工业大学 | Preparation method of silicon nitride @ silicon carbide @ boron nitride composite fiber felt |
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| US6040008A (en) * | 1997-08-04 | 2000-03-21 | University Of Florida | Silicon carbide fibers with boron nitride coatings |
| CN108385087A (en) * | 2018-02-12 | 2018-08-10 | 中南大学 | A method of it is continuous, quick to prepare SiC fiber surface BN coatings |
| CN109553430A (en) * | 2019-01-16 | 2019-04-02 | 苏州宏久航空防热材料科技有限公司 | A kind of SiC with compound interfacef/ SiC ceramic based composites and preparation method thereof |
| CN112624766A (en) * | 2020-12-29 | 2021-04-09 | 哈尔滨工业大学 | Preparation method of silicon nitride @ silicon carbide @ boron nitride composite fiber felt |
| CN116180451A (en) * | 2023-03-01 | 2023-05-30 | 湖南泽睿新材料有限公司 | A kind of continuous silicon carbide fiber sizing agent and its application |
| CN116903382A (en) * | 2023-07-21 | 2023-10-20 | 湖南泽睿新材料有限公司 | An equipment and method of rapidly depositing carbon coating on the surface of continuous silicon carbide fibers |
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