CN116986916A - Preparation device and preparation method of continuous chemical vapor deposition thick belt interface coating - Google Patents
Preparation device and preparation method of continuous chemical vapor deposition thick belt interface coating Download PDFInfo
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- CN116986916A CN116986916A CN202311254213.2A CN202311254213A CN116986916A CN 116986916 A CN116986916 A CN 116986916A CN 202311254213 A CN202311254213 A CN 202311254213A CN 116986916 A CN116986916 A CN 116986916A
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- 238000000576 coating method Methods 0.000 title claims abstract description 80
- 239000011248 coating agent Substances 0.000 title claims abstract description 76
- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 199
- 238000000151 deposition Methods 0.000 claims abstract description 178
- 230000008021 deposition Effects 0.000 claims abstract description 171
- 239000007789 gas Substances 0.000 claims abstract description 170
- 239000000835 fiber Substances 0.000 claims abstract description 124
- 238000009826 distribution Methods 0.000 claims abstract description 101
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 67
- 239000002243 precursor Substances 0.000 claims abstract description 49
- 238000010438 heat treatment Methods 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 30
- 238000001035 drying Methods 0.000 claims abstract description 20
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 65
- 238000007599 discharging Methods 0.000 claims description 6
- 239000004744 fabric Substances 0.000 claims description 6
- 229910003902 SiCl 4 Inorganic materials 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- 239000004917 carbon fiber Substances 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004804 winding Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 238000007789 sealing Methods 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910021389 graphene Inorganic materials 0.000 description 5
- 230000003068 static effect Effects 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000002905 metal composite material Substances 0.000 description 2
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 239000012783 reinforcing fiber Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 1
- 239000011153 ceramic matrix composite Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000011226 reinforced ceramic Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- 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
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62884—Coating the powders or the macroscopic reinforcing agents by gas phase techniques
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/46—Gases other than oxygen used as reactant, e.g. nitrogen used to make a nitride phase
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
Abstract
The invention discloses a preparation device and a preparation method of a continuous chemical vapor deposition thick belt interface coating. The method comprises the following steps: drying the thick fiber band, passing through the degumming module and the cavity, and introducing nitrogen into the cavity from the gas distribution box; introducing nitrogen into the cavity from the gas distribution box and the nitrogen inlet pipe, and heating the cavity and the degumming module; precursor gases are respectively introduced into the chamber from the two gas distribution boxes, so that the fiber thick belt continuously passes through the chamber; and closing the heating module and the degumming module, stopping introducing the precursor gas, and introducing nitrogen into the cavity from the gas distribution box and the nitrogen inlet pipe to obtain the continuous chemical vapor deposition thick-band interface coating. The invention can simultaneously improve the deposition efficiency and the thickness uniformity, so that the interface coating is deposited on each fiber yarn of the fiber thick belt.
Description
Technical Field
The invention belongs to the technical field of preparation of ceramic matrix composite interface coatings, and particularly relates to a preparation device and a preparation method of a continuous chemical vapor deposition thick belt interface coating.
Background
It is well known that in fiber reinforced ceramic matrix composites, the interfacial coating is one of the key components. The interface coating covers the surface of the reinforcing fiber, is connected with the reinforcing fiber and the ceramic matrix, plays roles in transferring and adjusting load and deflecting cracks, and directly influences the performance of the composite material. Chemical Vapor Deposition (CVD) processes are the most commonly used processes for preparing BN interface coatings, and can be classified into static CVD processes and continuous CVD processes according to the positional state of the workpiece at the time of deposition. The static CVD process is the most common preparation method of the CVD interface coating, namely, a base workpiece is kept in a deposition chamber during deposition, and is heated and insulated (deposited) together with equipment, and finally cooled and taken out; the continuous CVD process is an upgrade of the static CVD process, and in the CVD process, workpieces such as fibers, continuous belts and the like are continuously conveyed through an effective reaction area for deposition, so that the requirements of industrial production on high preparation efficiency and high consistency of interface coatings are met.
A major difficulty with CVD deposition of interfacial coatings is that it is not possible to combine the overall deposition efficiency with the internal and external uniformity of interfacial coating thickness. The reaction rate of the interface coating during deposition is controlled by the concentration of the precursor mixture, and the reaction rate affects the concentration gradient of the precursor mixture inside and outside the workpiece, so that if the overall deposition efficiency of the interface coating is to be accelerated, the concentration gradient of the two reaction gases in the workpiece is also increased, thereby causing the rapid increase of the thickness difference of the coating inside and outside the workpiece. Such detrimental phenomena are determined by the CVD deposition characteristics, resulting in a deterioration of the interface coating thickness non-uniformity in the workpiece; meanwhile, as the deposition speeds of the inner interface coating and the outer interface coating of the workpiece are different, the gap of the outer layer of the workpiece can be gradually blocked by the deposition coating along with the increase of the deposition time, precursor reactants are more difficult to diffuse into the workpiece, the problem of uneven thickness of the inner interface coating and the outer interface coating of the workpiece during deposition is further aggravated, and even unqualified products with hole sealing and crusting on the outer surface can be obtained under severe conditions.
In order to ensure the overall deposition efficiency to have practical value, the deposition speed of the continuous CVD process is far greater than that of the static CVD process, in which the residence time of the fiber or fiber unidirectional tape in the effective deposition area is usually several minutes, and the static CVD process is several hours, which makes the contradiction between the uniformity of the coating thickness and the deposition speed in the continuous CVD process particularly remarkable, and severely limits the application range of the continuous CVD deposition interface coating technology. In the prior art, the interface coating can be prepared on the single-bundle fibers by adopting a continuous CVD process, and continuous fiber braids such as fiber cloth, fiber felt and the like are thicker and more dense than the single-bundle fibers and are also more difficult to permeate, and if the continuous deposition method of the single-bundle fibers is simply applied, the effect is not ideal. In the range of deposition efficiency with practical value, the continuous CVD process in the prior art is difficult to prepare a qualified interface coating with uniform thickness, and even cannot be deposited at all, so that a preparation device and a preparation method for a continuous chemical vapor deposition interface coating are required to be developed to solve the problems in the prior art, and especially for preparing a thick fiber band interface coating with a thickness of more than 2mm.
The invention patent with application publication number of CN111058017A discloses a graphene metal composite wire and a low-temperature continuous preparation method thereof, wherein a wire is transported between a counter-roll input end and a counter-roll output end in a roll-to-roll deposition mode, a graphene layer is deposited on the surface of the wire in the wire transport process through a plasma enhanced chemical vapor deposition process, and the deposition temperature of the plasma enhanced chemical vapor deposition process is 700-850 ℃. According to the technical scheme, although the performance of the prepared graphene metal composite wire can be improved, the contradiction between the uniformity of the thickness of the graphene layer and the deposition speed in the continuous preparation process cannot be well controlled, so that the thickness of the graphene layer is uneven, and the product qualification rate is reduced.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation device for continuous chemical vapor deposition thick belt interface coating, which comprises a paying-off mechanism, a take-up mechanism, a deposition reaction chamber and a fiber thick belt, wherein the paying-off mechanism and the take-up mechanism are oppositely arranged; the preparation device also comprises a preheating degumming module, wherein the preheating degumming module is arranged between the paying-off mechanism and the deposition reaction chamber; a V-shaped structure is formed between the upper wall of the deposition reaction chamber and the lower wall of the deposition reaction chamber, the narrow end of the V-shaped structure is close to the paying-off mechanism, and the wide end of the V-shaped structure is close to the take-up mechanism; the thick fiber band sequentially horizontally passes through the preheating degumming module and the deposition reaction chamber, and the central axis of the thick fiber band, the central axis of the preheating degumming module and the central axis of the deposition reaction chamber coincide.
Preferably, an upper heating module is arranged on the outer side of the upper wall of the deposition reaction chamber, and a lower heating module is arranged on the outer side of the lower wall of the deposition reaction chamber.
In any of the above schemes, preferably, the fiber thick belt divides the deposition reaction chamber into two equal-volume upper chambers and lower chambers, the wide ends of the upper chambers and the lower chambers are respectively provided with a first gas distribution box and a second gas distribution box, and one side of the first gas distribution box and the second gas distribution box, which is connected with the deposition reaction chamber, is respectively and uniformly provided with a plurality of gas inlets; and the narrow end of the deposition reaction chamber is provided with an exhaust pipe, and the exhaust pipe is connected with the tail gas treatment device.
In any of the above schemes, it is preferable that the fiber thick belt is provided with a first group of nitrogen gas inlet pipes at the position of inputting the preheating degumming module, and the fiber thick belt is provided with a second group of nitrogen gas inlet pipes at the position of outputting the deposition reaction chamber; a first balance roller and a second balance roller are respectively arranged at the positions close to the first group of nitrogen inlet pipes and the second group of nitrogen inlet pipes; the first balance roller and the second balance roller are positioned on the same horizontal plane with the thick fiber band.
In any of the above aspects, it is preferable that the deposition reaction chamber is made of quartz or heat-resistant stainless steel material, and has a width equal to that of the thick fiber tape; the horizontal length of the deposition reaction chamber is 800-1500mm, the width of the deposition reaction chamber is 100-500mm, and the V-shaped included angle is 15-35 degrees; the length of the preheating degumming module is 30-50cm, and the width of the preheating degumming module is equal to the width of the thick fiber belt; the thick fiber band is a fiber woven cloth or a fiber felt composed of carbon fibers or silicon carbide fibers, and the thickness of the thick fiber band is more than 2mm. More preferably, the thickness of the fibrous thick band is expressed as h, and h is more than 2mm and less than or equal to 10mm.
The invention also provides a preparation method of the continuous chemical vapor deposition thick belt interface coating, which comprises the following steps in sequence by using the preparation device of the continuous chemical vapor deposition thick belt interface coating:
step one: placing a thick fiber tape to be deposited into a drying box for drying treatment, after the drying treatment is finished, installing the thick fiber tape on a paying-off mechanism, and pulling out the head of the thick fiber tape to enable the thick fiber tape to sequentially horizontally pass through a preheating degumming module and a deposition reaction chamber and be fixed on a wire collecting mechanism, wherein the central axis of the thick fiber tape, the central axis of the preheating degumming module and the central axis of the deposition reaction chamber coincide;
step two: introducing nitrogen into the deposition reaction chamber from the first gas distribution box and/or the second gas distribution box, and discharging air in the deposition reaction chamber;
step three: continuously introducing nitrogen into the deposition reaction chamber from the first gas distribution box and/or the second gas distribution box, and simultaneously introducing nitrogen into the deposition reaction chamber from the first group of nitrogen inlet pipes and the second group of nitrogen inlet pipes; starting a preheating degumming module to degumm and preheat, starting an upper heating module and a lower heating module to heat a deposition reaction chamber, and stopping introducing nitrogen into the deposition reaction chamber from the first gas distribution box and/or the second gas distribution box after the deposition reaction chamber is heated to a certain temperature;
step four: leading precursor gas into the deposition reaction chamber from the first gas distribution box and the second gas distribution box respectively, keeping nitrogen from the first group of nitrogen inlet pipes and the second group of nitrogen inlet pipes to be led into the deposition reaction chamber, and simultaneously starting the paying-off mechanism and the take-up mechanism to convey the fiber thick belt, so that the fiber thick belt continuously moves to sequentially pass through the preheating degumming module and the deposition reaction chamber to carry out continuous chemical vapor deposition, and simultaneously depositing the precursor gas on the upper surface and the lower surface of the fiber thick belt;
step five: after the continuous chemical vapor deposition is finished, closing the upper heating module, the lower heating module and the preheating degumming module, and simultaneously stopping introducing precursor gas into the deposition reaction chamber from the first gas distribution box and the second gas distribution box;
step six: and introducing nitrogen into the deposition reaction chamber from the first gas distribution box and/or the second gas distribution box, keeping introducing nitrogen into the deposition reaction chamber from the first group of nitrogen inlet pipes and the second group of nitrogen inlet pipes, and discharging precursor gas in the deposition reaction chamber, so that the continuous chemical vapor deposition thick-band interface coating can be obtained.
Preferably, in the first step, the drying temperature of the thick fiber band is 80-150 ℃ and the drying time is 1-2h.
In any of the above schemes, preferably, in the second step, the flow rate of the nitrogen gas introduced into the deposition reaction chamber from the first gas distribution box and/or the second gas distribution box is 1-5L/min, and the introduction time is 1-5h.
In any of the above schemes, preferably, in the third step, the flow rate of continuously introducing nitrogen into the deposition reaction chamber from the first gas distribution box and/or the second gas distribution box is 1-2L/min; the flow rate of nitrogen gas introduced into the deposition reaction cavity from the first group of nitrogen gas introducing pipes and the second group of nitrogen gas introducing pipes is 2-5L/min; the heating temperature of the preheating degumming module is 350-450 ℃; the heating process of the deposition reaction chamber is that the temperature is raised to 400 ℃ at the heating rate of 10-20 ℃/min, the temperature is kept for 30-60min, the temperature is continuously raised to 800 ℃ at the heating rate of 5-10 ℃/min, the temperature is kept for 30-60min, and the temperature is continuously raised to 1000 ℃ at the heating rate of 3-6 ℃/min.
In any of the above embodiments, preferably, in step four, whereThe precursor gas introduced into the first gas distribution box is BCl 3 Gas or SiCl 4 And H is 2 The SiCl 4 And H is 2 The mol ratio of the gas to the gas is 3:1, and the precursor gas introduced into the second gas separation box is NH 3 The method comprises the steps of carrying out a first treatment on the surface of the The flow rate of the precursor gas introduced into the first gas distribution box and the second gas distribution box is 300-1000ml/min; the flow rate of the nitrogen gas introduced into the first group of nitrogen gas introducing pipes and the second group of nitrogen gas introducing pipes is 1-2.5 times that of the precursor gas; the conveying speed of the fiber thick belt is 10-50cm/min.
In any of the above schemes, preferably, in the step six, the flow rate of nitrogen gas introduced into the deposition reaction chamber from the first gas distribution box and/or the second gas distribution box is 1-5L/min, and the flow rate of nitrogen gas introduced into the deposition reaction chamber from the first group of nitrogen gas introduction pipes and the second group of nitrogen gas introduction pipes is 1-5L/min.
In the invention, the two gas distribution boxes are adopted to carry out gas inlet layout on the input mode of the precursor gas, so that the input precursor gas is uniformly dispersed, the uniformity of the thickness of the thick-band interface coating of the fiber is improved, and the technical problems of uneven thickness of the interface coating, hole sealing and crusting even generated on the outer surface in the prior art are solved. The deposition reaction chamber with the V-shaped structure promotes the precursor gas to be forcedly permeated, improves the deposition efficiency and thickness uniformity, and solves the technical problems of slow permeation and diffusion, low deposition efficiency and the like of the precursor gas in the prior art. And nitrogen is simultaneously introduced into the first group of nitrogen inlet pipes and the second group of nitrogen inlet pipes in a nitrogen sealing mode, and excessive nitrogen is introduced to form nitrogen sealing at the position close to the fiber thick belt input and output deposition reaction chambers, so that reaction air is prevented from entering the deposition reaction chambers and reaction gas is prevented from leaving the deposition reaction chambers, and meanwhile, excessive nitrogen can dilute precursor gas in the deposition reaction chambers, so that precursor gas is dispersed more uniformly. The preheating degumming module is adopted to preheat the thick fiber belt, so that organic adhesive such as bundling agent and the like in the thick fiber belt is fully discharged.
The preparation device and the preparation method of the continuous chemical vapor deposition thick-band interface coating realize the preparation of the fiber thick-band interface coating with the thickness of more than 2mm by adopting a roll-to-roll continuous chemical vapor deposition process, adopt the forced permeation principle, uniformly deposit the interface coating on each fiber filament of the fiber woven cloth or the fiber felt, ensure the deposition efficiency and obtain the interface coating with better thickness consistency.
Drawings
FIG. 1 is a schematic view of a preferred embodiment of a continuous chemical vapor deposition thick interfacial coating manufacturing apparatus in accordance with the present invention;
FIG. 2 is a scanning electron microscope photograph of a deposited interfacial coating on a filament of a continuous chemical vapor deposited thick band interfacial coating prepared according to the embodiment of FIG. 1, in a position near the upper surface;
FIG. 3 is a scanning electron microscope photograph of a continuous chemical vapor deposited thick band interface coating prepared according to the embodiment of FIG. 1 deposited on a fiber at an intermediate location;
FIG. 4 is a scanning electron microscope photograph of a deposited interfacial coating on a filament of a continuous chemical vapor deposited thick band interfacial coating prepared according to the example shown in FIG. 1.
The reference numerals in the drawings indicate: the device comprises a 1-paying-off mechanism, a 2-winding mechanism, a 3-deposition reaction chamber, a 4-fiber thick belt, a 5-preheating degumming module, an upper wall of a 6-deposition reaction chamber, a lower wall of a 7-deposition reaction chamber, an 8-upper heating module, a 9-lower heating module, a 10-first gas distribution box, a 11-second gas distribution box, a 12-gas inlet hole, a 13-exhaust pipe, a 14-first group nitrogen gas inlet pipe, a 15-second group nitrogen gas inlet pipe, a 16-first balance roller and a 17-second balance roller.
Detailed Description
For a further understanding of the present invention, the present invention will be described in detail with reference to the following examples.
Embodiment one:
as shown in fig. 1, a preferred embodiment of the preparation device for continuous chemical vapor deposition thick belt interface coating according to the invention comprises a paying-off mechanism 1, a take-up mechanism 2, a deposition reaction chamber 3 and a thick fiber belt 4, wherein the paying-off mechanism 1 is opposite to the take-up mechanism 2, the deposition reaction chamber 3 is positioned at the middle position of the paying-off mechanism 1 and the take-up mechanism 2, the input end of the thick fiber belt 4 is wound on the paying-off mechanism 1, and the output end of the thick fiber belt 4 is wound on the take-up mechanism 2; the preparation device further comprises a preheating degumming module 5, wherein the preheating degumming module 5 is arranged between the paying-off mechanism 1 and the deposition reaction chamber 3; a V-shaped structure is formed between the upper wall 6 of the deposition reaction chamber and the lower wall 7 of the deposition reaction chamber, the narrow end of the V-shaped structure is close to the paying-off mechanism 1, and the wide end of the V-shaped structure is close to the take-up mechanism 2; the thick fiber band 4 sequentially horizontally passes through the preheating degumming module 5 and the deposition reaction chamber 3, and the central axis of the thick fiber band 4, the central axis of the preheating degumming module 5 and the central axis of the deposition reaction chamber 3 coincide.
An upper heating module 8 is arranged outside the upper wall 6 of the deposition reaction chamber, and a lower heating module 9 is arranged outside the lower wall 7 of the deposition reaction chamber. The fiber thick belt 4 divides the deposition reaction chamber 3 into two equal-volume upper chambers and lower chambers, the wide ends of the upper chambers and the lower chambers are respectively provided with a first gas distribution box 10 and a second gas distribution box 11, and a plurality of gas inlet holes 12 are respectively and uniformly arranged on one side of the first gas distribution box 10 and the second gas distribution box 11 connected with the deposition reaction chamber 3; an exhaust pipe 13 is arranged at the narrow end of the deposition reaction chamber 3, and the exhaust pipe 13 is connected with an exhaust gas treatment device.
The fiber thick belt 4 is provided with a first group of nitrogen gas inlet pipes 14 at the position of inputting the preheating degumming module 5, and the fiber thick belt 4 is provided with a second group of nitrogen gas inlet pipes 15 at the position of outputting the deposition reaction chamber 3; a first balance roller 16 and a second balance roller 17 are respectively arranged at the positions close to the first group of nitrogen gas inlet pipes 14 and the second group of nitrogen gas inlet pipes 15; the first counter-balance roller 16 and the second counter-balance roller 17 are on the same horizontal plane as the thick fibre strip 4.
The deposition reaction chamber 3 is made of quartz, and the width of the deposition reaction chamber is equal to that of the thick fiber belt 4; the horizontal length of the deposition reaction chamber 3 is 1200mm, the width is 300mm, and the V-shaped included angle is 25 degrees; the length of the preheating degumming module 5 is 40cm, and the width of the preheating degumming module is equal to the width of the thick fiber belt 4; the thick fiber band 4 is a fiber mat made of silicon carbide fibers, and has a thickness of 8mm.
The embodiment also provides a preparation method of the continuous chemical vapor deposition thick belt interface coating, which comprises the following steps in sequence by using the preparation device of the continuous chemical vapor deposition thick belt interface coating:
step one: placing a thick fiber tape to be deposited into a drying box for drying treatment, after the drying treatment is finished, installing the thick fiber tape on a paying-off mechanism, and pulling out the head of the thick fiber tape to enable the thick fiber tape to sequentially horizontally pass through a preheating degumming module and a deposition reaction chamber and be fixed on a wire collecting mechanism, wherein the central axis of the thick fiber tape, the central axis of the preheating degumming module and the central axis of the deposition reaction chamber coincide;
step two: introducing nitrogen into the deposition reaction chamber from the first gas distribution box and the second gas distribution box, and discharging air in the deposition reaction chamber;
step three: continuously introducing nitrogen into the deposition reaction chamber from the first gas distribution box and the second gas distribution box, and simultaneously introducing nitrogen into the deposition reaction chamber from the first group of nitrogen inlet pipes and the second group of nitrogen inlet pipes; starting a preheating degumming module to degumm and preheat, starting an upper heating module and a lower heating module to heat a deposition reaction chamber, and stopping introducing nitrogen into the deposition reaction chamber from a first gas distribution box and a second gas distribution box after the deposition reaction chamber is heated to a certain temperature;
step four: leading precursor gas into the deposition reaction chamber from the first gas distribution box and the second gas distribution box respectively, keeping nitrogen from the first group of nitrogen inlet pipes and the second group of nitrogen inlet pipes to be led into the deposition reaction chamber, and simultaneously starting the paying-off mechanism and the take-up mechanism to convey the fiber thick belt, so that the fiber thick belt continuously moves to sequentially pass through the preheating degumming module and the deposition reaction chamber to carry out continuous chemical vapor deposition, and simultaneously depositing the precursor gas on the upper surface and the lower surface of the fiber thick belt;
step five: after the continuous chemical vapor deposition is finished, closing the upper heating module, the lower heating module and the preheating degumming module, and simultaneously stopping introducing precursor gas into the deposition reaction chamber from the first gas distribution box and the second gas distribution box;
step six: and introducing nitrogen into the deposition reaction chamber from the first gas distribution box and the second gas distribution box, keeping introducing nitrogen into the deposition reaction chamber from the first group of nitrogen inlet pipes and the second group of nitrogen inlet pipes, and discharging precursor gas in the deposition reaction chamber, so that the continuous chemical vapor deposition thick-band interface coating can be obtained.
In the first step, the drying temperature of the thick fiber band is 120 ℃ and the drying time is 1.5h.
In the second step, the flow rate of nitrogen gas introduced into the deposition reaction chamber from the first gas distribution box and the second gas distribution box is 3L/min, and the introduction time is 3h.
Continuously introducing nitrogen into the deposition reaction chamber from the first gas distribution box and the second gas distribution box at a flow rate of 1.5L/min; the flow rate of nitrogen gas introduced into the deposition reaction chamber from the first group of nitrogen gas introduction pipes and the second group of nitrogen gas introduction pipes is 4L/min; the heating temperature of the preheating degumming module is 400 ℃; the heating process of the deposition reaction chamber is that the temperature is raised to 400 ℃ at a heating rate of 15 ℃/min, the temperature is kept for 45min, the temperature is continuously raised to 800 ℃ at a heating rate of 8 ℃/min, the temperature is kept for 45min, and the temperature is continuously raised to 1000 ℃ at a heating rate of 5 ℃/min.
In the fourth step, the precursor gas introduced into the first gas distribution box is BCl 3 The precursor gas introduced into the second gas separation box is NH 3 The method comprises the steps of carrying out a first treatment on the surface of the The flow rate of the precursor gas introduced into the first gas distribution box and the second gas distribution box is 700ml/min; the flow rate of the nitrogen gas introduced into the first group of nitrogen gas introducing pipes and the second group of nitrogen gas introducing pipes is 2 times that of the precursor gas, namely 1400ml/min; the conveying speed of the fiber thick belt is 30cm/min.
In the sixth step, the flow rate of nitrogen gas introduced into the deposition reaction chamber from the first gas distribution box and the second gas distribution box is 3L/min, and the flow rate of nitrogen gas introduced into the deposition reaction chamber from the first group of nitrogen gas introduction pipes and the second group of nitrogen gas introduction pipes is 3L/min.
In the embodiment, the two gas distribution boxes are adopted to perform gas inlet layout on the input mode of the precursor gas, so that the input precursor gas is uniformly dispersed, the uniformity of the thickness of the thick-band interface coating of the fiber is improved, and the technical problems of nonuniform thickness of the interface coating, hole sealing and crusting even generated on the outer surface in the prior art are solved. The deposition reaction chamber with the V-shaped structure promotes the precursor gas to be forcedly permeated, improves the deposition efficiency and thickness uniformity, and solves the technical problems of slow permeation and diffusion, low deposition efficiency and the like of the precursor gas in the prior art. And nitrogen is simultaneously introduced into the first group of nitrogen inlet pipes and the second group of nitrogen inlet pipes in a nitrogen sealing mode, and excessive nitrogen is introduced to form nitrogen sealing at the position close to the fiber thick belt input and output deposition reaction chambers, so that reaction air is prevented from entering the deposition reaction chambers and reaction gas is prevented from leaving the deposition reaction chambers, and meanwhile, excessive nitrogen can dilute precursor gas in the deposition reaction chambers, so that precursor gas is dispersed more uniformly. The preheating degumming module is adopted to preheat the thick fiber belt, so that organic adhesive such as bundling agent and the like in the thick fiber belt is fully discharged.
Scanning electron microscope pictures of the interfacial coating deposited on the fiber filaments near the upper surface, the middle position and the lower surface in the continuous chemical vapor deposition thick belt interfacial coating prepared in the embodiment are shown in fig. 2-4 respectively, wherein the thickness of the interfacial coating deposited on the fiber filaments near the upper surface is 227nm, the thickness of the interfacial coating deposited on the fiber filaments near the middle position is 161nm, and the thickness of the interfacial coating deposited on the fiber filaments near the lower surface is 196nm. As is apparent from FIGS. 2-4, the uniformity of the thickness of the interfacial coating at each part of the thick fiber tape is better, and the defects of hole sealing, crusting and the like are not generated on the outer surface.
The device and the method for preparing the thick-band interface coating by continuous chemical vapor deposition in the embodiment realize that the thick-band interface coating with the thickness exceeding 2mm is prepared by a roll-to-roll continuous chemical vapor deposition process, and adopt the forced permeation principle to uniformly deposit the interface coating on each fiber filament of the thick-band fiber, so that the interface coating with better thickness consistency can be obtained while the deposition efficiency is ensured.
Embodiment two:
according to another preferred embodiment of the apparatus for preparing a thick interfacial coating by continuous chemical vapor deposition and the preparation method thereof, the preparation apparatus, the preparation method, the technical principle, the beneficial effects and the like are basically the same as those of the first embodiment, except that:
preparation device for continuous chemical vapor deposition thick belt interface coating
The deposition reaction chamber is made of heat-resistant stainless steel, and the width of the deposition reaction chamber is equal to that of the thick fiber strip; the horizontal length of the deposition reaction chamber is 1500mm, the width of the deposition reaction chamber is 500mm, and the V-shaped included angle is 35 degrees; the length of the preheating degumming module is 50cm, and the width of the preheating degumming module is equal to the width of the thick fiber belt; the thick fiber band is a fiber woven cloth formed by carbon fibers, and the thickness of the thick fiber band is 10mm.
Preparation method for continuous chemical vapor deposition thick belt interface coating
In the first step, the drying temperature of the thick fiber band is 150 ℃ and the drying time is 1h.
In the second step, the flow rate of nitrogen gas introduced into the deposition reaction chamber from the first gas distribution box and the second gas distribution box is 5L/min, and the introduction time is 1h.
Continuously introducing nitrogen into the deposition reaction chamber from the first gas distribution box and the second gas distribution box at the flow rate of 2L/min; the flow rate of nitrogen gas introduced into the deposition reaction chamber from the first group of nitrogen gas introduction pipes and the second group of nitrogen gas introduction pipes is 5L/min; the heating temperature of the preheating degumming module is 450 ℃; the heating process of the deposition reaction chamber is that the temperature is raised to 400 ℃ at a heating rate of 20 ℃/min, the temperature is kept for 30min, the temperature is continuously raised to 800 ℃ at a heating rate of 10 ℃/min, the temperature is kept for 30min, and the temperature is continuously raised to 1000 ℃ at a heating rate of 6 ℃/min.
In the fourth stepThe precursor gas introduced into the first gas distribution box is BCl 3 The precursor gas introduced into the second gas separation box is NH 3 The method comprises the steps of carrying out a first treatment on the surface of the The flow rate of the precursor gas introduced into the first gas distribution box and the second gas distribution box is 1000ml/min; the flow rate of the nitrogen gas introduced into the first group of nitrogen gas introducing pipes and the second group of nitrogen gas introducing pipes is 1 time of the flow rate of the precursor gas, namely 1000ml/min; the conveying speed of the fiber thick belt is 50cm/min.
In the sixth step, the flow rate of nitrogen gas introduced into the deposition reaction chamber from the first gas distribution box and the second gas distribution box is 5L/min, and the flow rate of nitrogen gas introduced into the deposition reaction chamber from the first group of nitrogen gas introduction pipes and the second group of nitrogen gas introduction pipes is 5L/min.
Embodiment III:
according to another preferred embodiment of the apparatus for preparing a thick interfacial coating by continuous chemical vapor deposition and the preparation method thereof, the preparation apparatus, the preparation method, the technical principle, the beneficial effects and the like are basically the same as those of the first embodiment, except that:
(1) Preparation device for continuous chemical vapor deposition thick belt interface coating
The deposition reaction chamber is made of heat-resistant stainless steel, and the width of the deposition reaction chamber is equal to that of the thick fiber strip; the horizontal length of the deposition reaction chamber is 800mm, the width of the deposition reaction chamber is 100mm, and the V-shaped included angle is 15 degrees; the length of the preheating degumming module is 30cm, and the width of the preheating degumming module is equal to the width of the thick fiber belt; the thick fiber band is a fiber woven cloth formed by silicon carbide fibers, and the thickness of the thick fiber band is 4mm.
(2) Preparation method for continuous chemical vapor deposition thick belt interface coating
In the first step, the drying temperature of the thick fiber band is 80 ℃ and the drying time is 2 hours.
In the second step, the flow rate of nitrogen gas introduced into the deposition reaction chamber from the first gas distribution box and the second gas distribution box is 1L/min, and the introduction time is 5h.
Continuously introducing nitrogen into the deposition reaction chamber from the first gas distribution box and the second gas distribution box at the flow rate of 1L/min; the flow rate of nitrogen gas introduced into the deposition reaction chamber from the first group of nitrogen gas introduction pipes and the second group of nitrogen gas introduction pipes is 2L/min; the heating temperature of the preheating degumming module is 350 ℃; the heating process of the deposition reaction chamber is that the temperature is raised to 400 ℃ at the heating rate of 10 ℃/min, the temperature is kept for 60min, the temperature is continuously raised to 800 ℃ at the heating rate of 5 ℃/min, the temperature is kept for 60min, and the temperature is continuously raised to 1000 ℃ at the heating rate of 3 ℃/min.
In the fourth step, the precursor gas introduced into the first gas distribution box is SiCl 4 And H is 2 SiCl, of a mixture of (a) and (b) 4 And H is 2 The mol ratio of the gas to the gas is 3:1, and the precursor gas introduced into the second gas separation box is NH 3 The method comprises the steps of carrying out a first treatment on the surface of the The flow rate of the precursor gas introduced into the first gas distribution box and the second gas distribution box is 300ml/min; the flow rate of the nitrogen gas introduced into the first group of nitrogen gas introducing pipes and the second group of nitrogen gas introducing pipes is 2.5 times that of the precursor gas, namely 750ml/min; the conveying speed of the fiber thick belt is 10cm/min.
In the sixth step, the flow rate of nitrogen gas introduced into the deposition reaction chamber from the first gas distribution box and the second gas distribution box is 1L/min, and the flow rate of nitrogen gas introduced into the deposition reaction chamber from the first group of nitrogen gas introduction pipes and the second group of nitrogen gas introduction pipes is 1L/min.
The specific description is as follows: the technical scheme of the invention relates to a plurality of parameters, and the beneficial effects and remarkable progress of the invention can be obtained by comprehensively considering the synergistic effect among the parameters. In addition, the value ranges of all the parameters in the technical scheme are obtained through a large number of tests, and aiming at each parameter and the mutual combination of all the parameters, the inventor records a large number of test data, and the specific test data are not disclosed herein for a long period of time.
It will be appreciated by those skilled in the art that the apparatus and method for producing a continuous chemical vapor deposition thick interfacial coating of the present invention includes any combination of the above-described aspects of the invention and the detailed description of the invention and the parts shown in the drawings, and is limited in scope and does not describe each of these combinations for brevity. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The utility model provides a thick area interface coating's of continuous chemical vapor deposition preparation facilities, includes paying out machine constructs, admission machine constructs, deposit reaction chamber and thick area of fibre, paying out machine constructs with admission machine constructs the relative placement, deposit reaction chamber is located paying out machine constructs with admission machine constructs intermediate position, the thick area of fibre input winding is in on the admission machine constructs, the thick area of fibre output winding is in on the admission machine constructs, its characterized in that: the device also comprises a preheating degumming module, wherein the preheating degumming module is arranged between the paying-off mechanism and the deposition reaction chamber; a V-shaped structure is formed between the upper wall of the deposition reaction chamber and the lower wall of the deposition reaction chamber, the narrow end of the V-shaped structure is close to the paying-off mechanism, and the wide end of the V-shaped structure is close to the take-up mechanism; the thick fiber band sequentially horizontally passes through the preheating degumming module and the deposition reaction chamber, and the central axis of the thick fiber band, the central axis of the preheating degumming module and the central axis of the deposition reaction chamber coincide.
2. The apparatus for producing a thick interfacial coating by continuous chemical vapor deposition according to claim 1, wherein: an upper heating module is arranged on the outer side of the upper wall of the deposition reaction chamber, and a lower heating module is arranged on the outer side of the lower wall of the deposition reaction chamber.
3. The apparatus for producing a thick interfacial coating by continuous chemical vapor deposition according to claim 2, wherein: the fiber thick belt divides the deposition reaction chamber into two equal-volume upper chambers and lower chambers, the wide ends of the upper chambers and the lower chambers are respectively provided with a first gas distribution box and a second gas distribution box, and a plurality of gas inlets are uniformly arranged on one side, connected with the deposition reaction chamber, of the first gas distribution box and the second gas distribution box; and the narrow end of the deposition reaction chamber is provided with an exhaust pipe, and the exhaust pipe is connected with the tail gas treatment device.
4. The apparatus for producing a thick interfacial coating by continuous chemical vapor deposition according to claim 3, wherein: the fiber thick belt is provided with a first group of nitrogen gas inlet pipes at the position of inputting the preheating degumming module, and a second group of nitrogen gas inlet pipes at the position of outputting the deposition reaction chamber; a first balance roller and a second balance roller are respectively arranged at the positions close to the first group of nitrogen inlet pipes and the second group of nitrogen inlet pipes; the first balance roller and the second balance roller are positioned on the same horizontal plane with the thick fiber band.
5. The apparatus for producing a thick interfacial coating by continuous chemical vapor deposition according to claim 4, wherein: the deposition reaction chamber is made of quartz or heat-resistant stainless steel material, and the width of the deposition reaction chamber is equal to that of the thick fiber belt; the horizontal length of the deposition reaction chamber is 800-1500mm, the width of the deposition reaction chamber is 100-500mm, and the V-shaped included angle is 15-35 degrees; the length of the preheating degumming module is 30-50cm, and the width of the preheating degumming module is equal to the width of the thick fiber belt; the thick fiber band is a fiber woven cloth or a fiber felt composed of carbon fibers or silicon carbide fibers, and the thickness of the thick fiber band is more than 2mm.
6. A preparation method of a continuous chemical vapor deposition thick belt interface coating is characterized by comprising the following steps: the apparatus for producing a thick interfacial coating by continuous chemical vapor deposition according to any one of claims 1 to 5, comprising the steps of,
step one: placing a thick fiber tape to be deposited into a drying box for drying treatment, after the drying treatment is finished, installing the thick fiber tape on a paying-off mechanism, and pulling out the head of the thick fiber tape to enable the thick fiber tape to sequentially horizontally pass through a preheating degumming module and a deposition reaction chamber and be fixed on a wire collecting mechanism, wherein the central axis of the thick fiber tape, the central axis of the preheating degumming module and the central axis of the deposition reaction chamber coincide;
step two: introducing nitrogen into the deposition reaction chamber from the first gas distribution box and/or the second gas distribution box, and discharging air in the deposition reaction chamber;
step three: continuously introducing nitrogen into the deposition reaction chamber from the first gas distribution box and/or the second gas distribution box, and simultaneously introducing nitrogen into the deposition reaction chamber from the first group of nitrogen inlet pipes and the second group of nitrogen inlet pipes; starting a preheating degumming module to degumm and preheat, starting an upper heating module and a lower heating module to heat a deposition reaction chamber, and stopping introducing nitrogen into the deposition reaction chamber from the first gas distribution box and/or the second gas distribution box after the deposition reaction chamber is heated to a certain temperature;
step four: leading precursor gas into the deposition reaction chamber from the first gas distribution box and the second gas distribution box respectively, keeping nitrogen from the first group of nitrogen inlet pipes and the second group of nitrogen inlet pipes to be led into the deposition reaction chamber, and simultaneously starting the paying-off mechanism and the take-up mechanism to convey the fiber thick belt, so that the fiber thick belt continuously moves to sequentially pass through the preheating degumming module and the deposition reaction chamber to carry out continuous chemical vapor deposition, and simultaneously depositing the precursor gas on the upper surface and the lower surface of the fiber thick belt;
step five: after the continuous chemical vapor deposition is finished, closing the upper heating module, the lower heating module and the preheating degumming module, and simultaneously stopping introducing precursor gas into the deposition reaction chamber from the first gas distribution box and the second gas distribution box;
step six: and introducing nitrogen into the deposition reaction chamber from the first gas distribution box and/or the second gas distribution box, keeping introducing nitrogen into the deposition reaction chamber from the first group of nitrogen inlet pipes and the second group of nitrogen inlet pipes, and discharging precursor gas in the deposition reaction chamber, so that the continuous chemical vapor deposition thick-band interface coating can be obtained.
7. The method for preparing the continuous chemical vapor deposition thick belt interface coating according to claim 6, wherein: in the first step, the drying temperature of the thick fiber band is 80-150 ℃ and the drying time is 1-2h; in the second step, the flow rate of nitrogen gas introduced into the deposition reaction chamber from the first gas distribution box and/or the second gas distribution box is 1-5L/min, and the introduction time is 1-5h.
8. The method for preparing the continuous chemical vapor deposition thick belt interface coating according to claim 7, wherein: continuously introducing nitrogen into the deposition reaction chamber from the first gas distribution box and/or the second gas distribution box at a flow rate of 1-2L/min; the flow rate of nitrogen gas introduced into the deposition reaction cavity from the first group of nitrogen gas introducing pipes and the second group of nitrogen gas introducing pipes is 2-5L/min; the heating temperature of the preheating degumming module is 350-450 ℃; the heating process of the deposition reaction chamber is that the temperature is raised to 400 ℃ at the heating rate of 10-20 ℃/min, the temperature is kept for 30-60min, the temperature is continuously raised to 800 ℃ at the heating rate of 5-10 ℃/min, the temperature is kept for 30-60min, and the temperature is continuously raised to 1000 ℃ at the heating rate of 3-6 ℃/min.
9. The method for preparing the continuous chemical vapor deposition thick belt interface coating according to claim 8, wherein: in the fourth step, the precursor gas introduced into the first gas distribution box is BCl 3 Gas or SiCl 4 And H is 2 The SiCl 4 And H is 2 The mol ratio of the gas to the gas is 3:1, and the precursor gas introduced into the second gas separation box is NH 3 The method comprises the steps of carrying out a first treatment on the surface of the The flow rate of the precursor gas introduced into the first gas distribution box and the second gas distribution box is 300-1000ml/min; the flow rate of the nitrogen gas introduced into the first group of nitrogen gas introducing pipes and the second group of nitrogen gas introducing pipes is 1-2.5 times that of the precursor gas; the conveying speed of the fiber thick belt is 10-50cm/min.
10. The method for preparing the continuous chemical vapor deposition thick belt interface coating according to claim 9, wherein: in the sixth step, the flow rate of nitrogen gas introduced into the deposition reaction chamber from the first gas distribution box and/or the second gas distribution box is 1-5L/min, and the flow rate of nitrogen gas introduced into the deposition reaction chamber from the first group of nitrogen gas introducing pipes and the second group of nitrogen gas introducing pipes is 1-5L/min.
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