CN111172519A - Device and method for continuously preparing composite interface layer on surface of silicon carbide fiber - Google Patents
Device and method for continuously preparing composite interface layer on surface of silicon carbide fiber Download PDFInfo
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- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/32—Carbides
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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- C23C16/342—Boron nitride
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
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Abstract
The invention relates to a device and a method for continuously preparing a composite interface layer on the surface of silicon carbide fiber, wherein the device comprises a first deposition chamber and at least one transitional deposition chamber, an isolation chamber is arranged between any two adjacent deposition chambers, inert gas is introduced into the isolation chamber, and the gas pressure of the inert gas in the isolation chamber is higher than the indoor gas pressure of the two adjacent deposition chambers, so that the gases in the two adjacent deposition chambers are isolated from each other under the action of the gas pressure difference and cannot flow into the isolation chamber; each deposition chamber is provided with a roller group for guiding the fiber bundle. The invention solves the following problems: the interface layer is deposited in batches, and the thickness of the interface layer of different furnaces of the same furnace are difficult to realize uniformity. The SiC fibers are heated and cooled along with the furnace body during each heat deposition, the treatment time at high temperature is too long, the fiber strength is obviously reduced, and the like.
Description
Technical Field
The invention relates to the field of ceramic matrix composite materials, in particular to equipment and a method for continuously preparing a composite interface layer on the surface of bundled silicon carbide fiber based on CVD (chemical vapor deposition), and belongs to the field of composite materials.
Background
SiC-based composite material (SiC) toughened by continuous SiC fibersfthe/SiC composite material) is a material which takes SiC fibers as a reinforcing phase and takes SiC ceramics as a matrix, has the advantages of high temperature resistance, low density, oxidation resistance, insensitivity to cracks, difficult occurrence of catastrophic fracture and the like, and thus has wide application in the fields of aerospace and the like. The preparation process of the material mainly comprises a chemical vapor infiltration method, a polymer impregnation-pyrolysis method, an infiltration method, a nano impregnation and transient eutectic method and the like. In addition to the chemical vapor infiltration method, other methods need to prepare an interface layer on the surface of the bundle fiber SiC fiber in advance, and the most common preparation method of the interface layer is chemical vapor deposition/infiltration (CVD/CVI). In general terms, chemical vapor infiltration processes are at lower pressures than chemical vapor deposition processes, and are more conducive to diffusion of the reactive atmosphere within the fabric and within the fiber bundle.The interfacial layer being SiCfAn indispensable part of the/SiC composite material. The interface layer converts strong bonding between the fiber and the matrix into weak bonding through the action of crack deflection and crack blocking, so that the ceramic, which is the traditional brittle material, can form a ceramic matrix composite with toughness. The performance of the interface layer is improved by SiCfThe key of the mechanical property of the/SiC composite material.
In recent years, continuous interfacial layer deposition techniques have attracted attention, for example, the invention patent application CN108385087A of crabapple, yang, reports a method for continuously and rapidly preparing Boron Nitride (BN) interfacial layers on the surface of SiC fibers, and the US patent application US2018/0347106a1 of buete, et al, reports a general apparatus for depositing an interfacial layer on one or more bundles of filament fibers. On the other hand, the continuous graphitization treatment of the carbon fiber is a relatively mature technology and can provide reference for the heat treatment of the silicon carbide fiber with the interface layer. However, SiCfthe/SiC composite material needs a composite interface layer. If the process of winding and unwinding and startup and shutdown is carried out once for each treatment, not only are the mechanical damage and the thermal damage caused to the fibers large, but also the precious time is wasted. Thus, U.S. patent application US2018/0347048a1 to Buet e. However, this device has two disadvantages: different deposition atmospheres can mutually pollute through micropore diffusion, and the quality of an interface layer is influenced; all deposition zones have the same temperature, which limits the flexibility of the preparation process of different interface layers.
Disclosure of Invention
The technical problem solved by the invention is as follows: (1) the interface layer is deposited in batches, and the thickness of the interface layer of different furnaces of the same furnace are difficult to realize uniformity.
(2) During each heat deposition, the SiC fibers are heated and cooled along with the furnace body, the treatment time is too long at high temperature, and the fiber strength is obviously reduced.
The technical scheme of the invention is as follows:
providing equipment for continuously preparing a composite interface layer on the surface of silicon carbide fiber, wherein the equipment comprises a first deposition chamber and at least one transitional deposition chamber, an isolation chamber is arranged between any two adjacent deposition chambers, inert gas is introduced into the isolation chamber, and the gas pressure of the inert gas in the isolation chamber is higher than the indoor gas pressure of the two adjacent deposition chambers, so that the gases in the two adjacent deposition chambers are isolated from each other under the action of the gas pressure difference and cannot flow into the isolation chamber; each deposition chamber is provided with a roller group for guiding the fiber bundle.
The equipment comprises a first deposition chamber, at least one transition deposition chamber and a heat treatment chamber, wherein the first deposition chamber, the at least one transition deposition chamber and the heat treatment chamber are sequentially arranged, an isolation chamber is arranged between any two adjacent deposition chambers, an isolation chamber is arranged between the transition deposition chamber and the heat treatment chamber, inert gas is introduced into the isolation chamber, and the gas pressure of the inert gas in the isolation chamber is higher than the indoor gas pressure of the two adjacent chambers, so that the gases in the two adjacent chambers are isolated from each other under the action of the gas pressure difference and cannot flow into the isolation chamber; each deposition chamber is provided with a roller group for guiding the fiber bundle;
and a material receiving device is arranged in the heat treatment chamber and used for pulling the fiber bundle and winding the fiber bundle.
Furthermore, a discharging device and a fiber material roll are arranged in the first deposition chamber, and the fiber material roll is arranged on the discharging device.
Furthermore, a material receiving device is arranged in the transition deposition chamber at the tail end and used for pulling the fiber bundle and winding the fiber bundle.
Further, the inert gas is argon (Ar).
Furthermore, the air pressure in the isolation chamber is 300 Pa-1 kPa higher than that of the adjacent deposition chamber.
Furthermore, a steering roller is arranged in at least one deposition chamber, and the beam wires in the deposition chamber are guided out from the inlet of the deposition chamber after being steered by the steering roller. The length of the deposition chamber is halved by arranging the steering rollers, so that the space and the energy consumption are saved.
Further, the first deposition chamber comprises a turning roller, and the bundled SiC fibers are turned by the turning roller after entering the first deposition chamber.
Further, the transitional deposition chamber comprises a steering roller, and the bundled SiC fibers are steered by the steering roller after entering the transitional deposition chamber.
Furthermore, the wall of the deposition chamber is made of quartz.
There is provided a method for continuously preparing a composite interface layer, using the above apparatus for continuously preparing a composite interface layer, the method comprising the steps of:
step 1, pre-winding a bundle wire SiC fiber on a roller, enabling the bundle wire SiC fiber to enter a first deposition chamber, and depositing in the first deposition chamber to form a first interface layer;
and 2, enabling the bundled SiC fibers to enter at least one transitional deposition chamber, and depositing in the transitional deposition chamber to form at least one interface layer.
Further, the bundle silk SiC fiber enters a heat treatment chamber, and the crystallinity of the interface layer is improved through heat treatment. Preferably, the heating temperature of all the deposition chambers is not higher than 1000 ℃, and the heat treatment temperature of the heat treatment chamber is above 1000 ℃.
The invention has the advantages that: (1) the device can continuously and rapidly deposit the composite interface layer, thereby saving the preparation time to the maximum extent and reducing the energy consumption. The composite interfacial layer may be pyrolytic carbon (PyC), Boron Nitride (BN), silicon carbide (SiC), silicon nitride (Si)3N4) One or a combination of a plurality of mixed interface layers of silicon-doped boron nitride, boron-doped silicon nitride, boron-doped pyrolytic carbon and the like,
(2) the deposition atmosphere, temperature and pressure experienced by each section of fiber of the device are almost the same, and the uniformity and consistency of the composite interface layer are improved to the maximum extent.
(3) The temperature, pressure and atmosphere of each deposition chamber of the device can be independently controlled, and the uniformity of interface layer deposition is improved. The deposition chamber is separated by an isolation chamber with high pressure, the deposition atmosphere does not pollute each other, and the purity of each interface layer is ensured.
(4) The tail gas generated by each deposition chamber of the device can be independently and pertinently treated, so that the safety and the environmental friendliness of the deposition process are improved, and the service lives of the vacuum pump set and the tail gas treatment system are prolonged.
(5) The deposition temperature of each interface layer of the device is below 1000 ℃, so that the chemical reaction is mild, and the thickness of the interface layer on the surface of each monofilament in the bundle is uniform and controllable.
(6) Through final rapid and continuous heat treatment, the crystallinity of the interface layer is improved, the performance of the interface layer is improved, the fiber is protected to the maximum extent, and the heat damage of the fiber is reduced.
(7) The lower deposition temperature allows the deposition chamber to be made of quartz, and the material has the advantages of accurate forming size, good airtightness and low price. The lengths, pipe diameters and the like of the deposition chamber and the heating body can be freely adjusted and combined, composite interface layers with rich types can be deposited, and the deposition process adjusting range of each interface layer is large.
Drawings
FIG. 1 is a schematic view of the apparatus of the present invention (the last chamber is a thermal processing chamber).
FIG. 2 is a schematic view of the apparatus of the present invention (the last chamber being a transitional deposition chamber).
1 a first deposition chamber, 2 a transition deposition chamber, 3 a heat treatment chamber, 4 an isolation chamber, 5 roller groups, 6a discharging device and a fiber material roll, 7a fiber bundle, 8a receiving device and 9 a steering roller.
Detailed Description
The present invention is described in further detail below.
Example 1: this example prepares a PyC/BN/SiC composite interfacial layer, the apparatus comprising a first deposition chamber, a transitional deposition chamber, a thermal treatment chamber, etc. Depositing a PyC interface layer in a first deposition chamber by using a phi 80 quartz tube, wherein the length of a constant temperature region is 300mm, the temperature is 1000 ℃, and the pressure is 500 Pa; the transition deposition chamber 1 is used for depositing a BN interface layer, a phi 100 quartz tube is adopted, the temperature is 1000 ℃, the length of a constant temperature zone is 600mm, and the pressure is 100 Pa. The transitional deposition chamber 2 deposits a SiC interface layer, and adopts a phi 120 quartz tube, the temperature is 900 ℃, the length of a constant temperature region is 500mm, and the pressure is 1000 Pa. The heat treatment chamber adopts a water-cooled steel furnace, a graphite muffle with the diameter of phi 120, the length of a constant temperature zone of 600mm, the temperature of 1800 ℃ and the pressure of 2000 Pa.
After the SiC fibers subjected to sizing agent removal are subjected to carbon fiber traction and filament hanging, the equipment is vacuumized, and the furnace is washed for 3 times by Ar. And starting a heating device, heating the first deposition chamber to 1000 ℃, heating the transitional deposition chamber 1 to 1000 ℃, and heating the transitional deposition chamber 2 to 900 ℃. After keeping the temperature for 30min, introducing Ar from a protective gas inlet at the flow rate of 3L/min. Feeding propane (C) to the first deposition chamber3H8) And Ar, the intake rates of which are 0.2L/min and 1.8L/min, respectively. Introducing gas into the transitional deposition chamber 1 in two paths, wherein one path is ammonia gas (NH)32L/min), and the other is boron trichloride (BCl)30.4L/min) and hydrogen (H)22L/min). Trichloromethylsilane (MTS) and H were fed into the intermediate deposition chamber 32Wherein the flow rate of MTS is 1.5g/min, H2The flow rate was 2L/min. And adjusting the valve opening degree of the reaction gas exhaust port and the valve opening degree of the protective gas exhaust port, and controlling the pressure of the isolation chamber to be 2000Pa, the pressure of the first deposition chamber to be 500Pa, the pressure of the transitional deposition chamber 1 to be 100Pa and the pressure of the transitional deposition chamber 2 to be 1000 Pa. And starting a filament collecting motor while introducing reaction gas, and adjusting the filament collecting speed to be 0.8 cm/min. The average thickness of the PyC interface layer was 100nm, the average thickness of the BN interface layer was 500nm, and the average thickness of the SiC interface layer was 300 nm.
Example 2: this example prepares a BN/boron-doped silicon nitride composite interfacial layer. The apparatus includes a first deposition chamber, a transitional deposition chamber, a thermal processing chamber, and the like. Preparing a BN interface layer in a first deposition chamber by using a phi 80 quartz tube, wherein the length of a constant temperature region is 600mm, the temperature is 900 ℃, and the pressure is 500 Pa; preparing a boron-doped silicon nitride interface layer in a transitional deposition chamber by adopting a phi 100 quartz tube, wherein the length of a constant temperature region is 500mm, the temperature is 1000 ℃, and the pressure is 100 Pa; the heat treatment chamber adopts a water-cooled steel furnace, a graphite muffle with the diameter of phi 120, the length of a constant temperature zone of 600mm, the temperature of 1800 ℃ and the pressure of 2000 Pa.
After the SiC fibers subjected to sizing agent removal are subjected to carbon fiber traction and filament hanging, the equipment is vacuumized, and the furnace is washed for 3 times by Ar. And starting a heating device, heating the first deposition chamber to 900 ℃, heating the transition deposition chamber to 1000 ℃, and heating the heat treatment chamber to 1800 ℃. After keeping the temperature for 30min, introducing Ar from a protective gas inlet at the flow rate of 3L/min. Introducing gas into the first deposition chamber in two paths, wherein one path is NH3(2L/min), the other is BCl3(0.5L/min) and H2(3L/min). Introducing air into the transitional deposition chamber in two ways, wherein one way is BCl3(0.05L/min), Silicachloroform (SiHCl)30.2L/min) and H2(3L/min), the other is NH3(1L/min). The valve opening degree of the reaction gas exhaust port and the valve opening degree of the protective gas exhaust port are adjusted, the pressure of the isolation chamber is controlled to be 2000Pa, the pressure of the first deposition chamber is controlled to be 500Pa, the pressure of the transition deposition chamber is controlled to be 100Pa, and the pressure of the heat treatment chamber is controlled to be 2000 Pa. And starting a filament collecting motor while introducing reaction gas, and adjusting the filament collecting speed to be 1.0 cm/min. The average thickness of the obtained BN interface layer is 500nm, the average thickness of the obtained boron-doped silicon nitride interface layer is 200nm, the boron-silicon atomic ratio is about 1: 4.
Claims (10)
1. the equipment for continuously preparing the composite interface layer on the surface of the silicon carbide fiber comprises a first deposition chamber and at least one transitional deposition chamber, wherein an isolation chamber is arranged between any two adjacent deposition chambers, inert gas is introduced into the isolation chamber, and the gas pressure of the inert gas in the isolation chamber is higher than the indoor gas pressure of the two adjacent deposition chambers, so that the gases in the two adjacent deposition chambers are isolated from each other under the action of the gas pressure difference and cannot flow into the isolation chamber; each deposition chamber is provided with a roller group for guiding the fiber bundle.
2. The equipment for continuously preparing the composite interface layer on the surface of the silicon carbide fiber comprises a first deposition chamber, at least one transition deposition chamber and a heat treatment chamber, wherein the first deposition chamber, the at least one transition deposition chamber and the heat treatment chamber are sequentially arranged, an isolation chamber is arranged between any two adjacent deposition chambers, an isolation chamber is arranged between the transition deposition chamber and the heat treatment chamber, inert gas is introduced into the isolation chamber, and the gas pressure of the inert gas in the isolation chamber is higher than the indoor gas pressure of the two adjacent chambers, so that the gases in the two adjacent chambers are isolated from each other under the action of the gas pressure difference and cannot flow into the isolation chamber; each deposition chamber is provided with a roller group for guiding the fiber bundle;
and a material receiving device is arranged in the heat treatment chamber and used for pulling the fiber bundle and winding the fiber bundle.
3. The apparatus for continuously preparing the composite interface layer on the surface of the silicon carbide fiber according to claim 1 or 2, wherein: the first deposition chamber is internally provided with a discharging device and a fiber material roll, and the fiber material roll is arranged on the discharging device.
4. The apparatus for continuously preparing the composite interface layer on the surface of the silicon carbide fiber according to claim 1 or 2, wherein: and a material receiving device is arranged in the transition deposition chamber at the tail end and used for pulling the fiber bundle and winding the fiber bundle.
5. The apparatus for continuously preparing the composite interface layer on the surface of the silicon carbide fiber according to claim 1 or 2, wherein: the inert gas is argon (Ar).
6. The apparatus for continuously preparing the composite interface layer on the surface of the silicon carbide fiber according to claim 1 or 2, wherein: the air pressure in the isolation chamber is 300 Pa-1 kPa higher than that of the adjacent deposition chamber.
7. The apparatus for continuously preparing the composite interface layer on the surface of the silicon carbide fiber according to claim 1 or 2, wherein: and a steering roller is arranged in at least one deposition chamber, and the beam wires in the deposition chamber are steered by the steering roller and then are led out from the inlet of the deposition chamber. The length of the deposition chamber is halved by arranging the steering rollers, so that the space and the energy consumption are saved.
8. The apparatus for continuously preparing the composite interface layer on the surface of the silicon carbide fiber according to claim 1 or 2, wherein: the first deposition chamber comprises a steering roller, and the bundled SiC fibers are steered through the steering roller after entering the first deposition chamber; the transitional deposition chamber comprises a steering roller, and the bundled SiC fibers are steered through the steering roller after entering the transitional deposition chamber.
9. There is provided a method of continuously preparing a composite interface layer using the apparatus for continuously preparing a composite interface layer according to any one of claims 1 to 8, the method comprising the steps of:
step 1, pre-winding a bundle wire SiC fiber on a roller, enabling the bundle wire SiC fiber to enter a first deposition chamber, and depositing in the first deposition chamber to form a first interface layer;
and 2, enabling the bundled SiC fibers to enter at least one transitional deposition chamber, and depositing in the transitional deposition chamber to form at least one interface layer.
10. The method of claim 9, wherein the method comprises the steps of: and the bundled SiC fibers enter a heat treatment chamber, and the crystallinity of the interface layer is improved through heat treatment. Preferably, the heating temperature of all the deposition chambers is not higher than 1000 ℃, and the heat treatment temperature of the heat treatment chamber is above 1000 ℃.
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| CN115404465A (en) * | 2021-05-26 | 2022-11-29 | 中国科学院上海硅酸盐研究所 | Equipment and method for preparing composite interface on surface of continuous fiber |
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