CN114134484B - Vortex auxiliary system and method for preparing fiber reinforced composite material by chemical vapor infiltration method - Google Patents
Vortex auxiliary system and method for preparing fiber reinforced composite material by chemical vapor infiltration method Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 50
- 230000008595 infiltration Effects 0.000 title claims abstract description 30
- 238000001764 infiltration Methods 0.000 title claims abstract description 30
- 239000000463 material Substances 0.000 title claims abstract description 28
- 239000000126 substance Substances 0.000 title claims abstract description 26
- 239000003733 fiber-reinforced composite Substances 0.000 title claims abstract description 15
- 239000002131 composite material Substances 0.000 claims abstract description 52
- 230000008021 deposition Effects 0.000 claims abstract description 44
- 238000000280 densification Methods 0.000 claims abstract description 30
- 238000009792 diffusion process Methods 0.000 claims abstract description 29
- 238000007789 sealing Methods 0.000 claims abstract description 11
- 238000000151 deposition Methods 0.000 claims description 52
- 239000007789 gas Substances 0.000 claims description 51
- 229910004009 SiCy Inorganic materials 0.000 claims description 22
- 239000001257 hydrogen Substances 0.000 claims description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims description 18
- 239000000835 fiber Substances 0.000 claims description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- 239000012530 fluid Substances 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 12
- 150000002431 hydrogen Chemical class 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 10
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 238000005137 deposition process Methods 0.000 claims description 4
- 238000010297 mechanical methods and process Methods 0.000 claims description 3
- 239000002344 surface layer Substances 0.000 claims description 3
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- 238000002360 preparation method Methods 0.000 abstract description 17
- 239000011153 ceramic matrix composite Substances 0.000 abstract description 12
- 238000012545 processing Methods 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 description 11
- 239000011148 porous material Substances 0.000 description 6
- 239000012495 reaction gas Substances 0.000 description 5
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- 230000035515 penetration Effects 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 238000009417 prefabrication Methods 0.000 description 1
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- 239000011226 reinforced ceramic Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C16/325—Silicon carbide
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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
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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- 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
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- 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
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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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- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
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- 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
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
Abstract
The invention relates to an eddy current auxiliary system for preparing a fiber reinforced composite material by a chemical vapor infiltration method and a preparation method thereof. So that the gas diffusion dynamics during densification have a vortex flow diffusion dynamics. Meanwhile, the mode of removing the outer hole sealing layer by mechanical processing is adopted in addition to the vortex auxiliary deposition mode, so that the compactness and the density uniformity of the composite material prepared by CVI are improved, the diffusion depth of about 10mm can be realized, the preparation of the large-size ceramic matrix composite material is realized, and the relative density is more than 90%.
Description
Technical Field
The invention belongs to the field of Chemical Vapor Infiltration (CVI) preparation in the field of ceramic matrix composite materials, and relates to a vortex auxiliary system for preparing a fiber reinforced composite material by a chemical vapor infiltration method and a preparation method. In the preparation of ceramic matrix composites using conventional CVI methods, reactant gases are introduced into the deposition chamber by creating an inner and outer vortex layer that provides an initial velocity of movement of the gases into the fiber preform as it passes over the surface. So that the gas diffusion power in the densification process has the power of vortex flow diffusion besides the conventional concentration diffusion. By the method, not only the compactness and density uniformity of the composite material prepared by CVI are improved, but also the diffusion depth of about 10mm can be realized, and the preparation of the large-size ceramic matrix composite material is realized.
Background
With the widespread use of ceramic matrix composites in the aerospace field, an increasing number of large components need to be replaced with them. The thickness of the ceramic matrix composite material prepared by the traditional CVI method is limited (2 mm-5 mm), and the application field of the composite material is limited.
The frock that traditional CVI method used is generally box, and there is even rectification gas pocket parallel arrangement at the bottom of the case, carries out vertical placement with panel at the position that does not have the hole, makes the reaction air supply can pass through the panel at the uniform velocity parallel, forms the laminar flow, relies on the concentration difference that gas itself exists in the fibre prefabrication body surface to carry out vertical concentration diffusion infiltration. The traditional laminar flow uniform hole die rectifying mode cannot be used for depositing a cylindrical sample with higher thickness, and premature hole sealing time, technological parameters difficult to adjust and the like can negatively influence the CVI process. Resulting in a penetration depth of only 2 to 5mm in this way.
Chinese patent application CN 105367105a discloses a method for preparing thick-wall ceramic matrix composite by mechanical processing assisted CVI, which enlarges the diffusion mass transfer channel of air flow by drilling in the thickness direction of the sample, so as to achieve the purpose of increasing the thickness of the sample (greater than 5 mm), but the method damages the integrity of the ceramic matrix composite, and cannot meet the preparation of large-scale components. Chinese patent application CN111574237a discloses an oversized carbon/carbon composite sheet and equipment for its preparation. The pore plate is used for adjusting the gas inlet to realize the adjustment of the deposition process and the preparation of the special-shaped piece. However, the deposition is still carried out in a laminar flow mode after the gas is introduced, and dead angles are easy to exist. Chinese patent application CN 111170751A discloses a CVI densification method for large wall thickness ceramic matrix composite parts, which introduces pilot holes into the densification process, by repeatedly machining the pilot holes along the depth and matching with long densification, thicker components (greater than 6 mm) can be produced. Although the subsequent pilot holes may be filled with fibers and densified, drilling may still compromise the integrity of the original preform physical properties.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a vortex auxiliary system for preparing a fiber reinforced composite material by a chemical vapor infiltration method and a preparation method thereof.
In order to overcome the defects in the prior art, the invention provides a vortex auxiliary system and a vortex auxiliary method for chemical vapor infiltration densification of a fiber reinforced composite material. The system abandons uniform and uniform flow holes of the traditional CVI, uses a pair of inner vortex air inlet channels and outer vortex air inlet channels, and divides and merges internal fluid and constructs vortex by adjusting blades so that the air flow has a trend of moving inwards from the surface of the fiber preform. The die system can form a new diffusion mode of 'flow diffusion' besides the dynamic diffusion mode of 'concentration diffusion'. When the eddy current has the horizontal velocity, the gas can effectively permeate the hollow cylindrical sample, the permeation depth (the wall thickness is more than 10 mm) is increased, and the deposition efficiency of the composite material is improved, so that a more complex barrel-shaped sample can be prepared.
Meanwhile, as an auxiliary vortex platform (see fig. 3) of the die core, an inner vortex air inlet channel and an outer vortex air inlet channel are formed in pairs, the total number of channels n is even and n/2>1, and the number of regulating blades j=n/2. The air flow is split into two paths at the platform. The first path passes through the inner vortex air inlet channel, and spirally rises to flow through the inner wall of the sample after being regulated by the regulating blade. The second path passes through the outer vortex air inlet channel, and spirally rises to flow through the outer wall of the sample after passing through the outer wall of the adjusting blade.
Wherein the die land channel diameter has the following mathematical relationship with vent holes (sizing see fig. 3):
R 2 ＝15.6r 2
wherein r is an internal and external vortex air inlet channelRadius. R is the radius of the inner hole of the sample cylinder. d, d 0 For the width of the outer vortex channel d 1 For the width of the outlet of the internal and external vortex channels, d 2 Is the width of the inner vortex channel. i is the length of the vortex tail wing in the adjusting blade, and n is the total number of vortex channels.
The mathematical relationship is mainly used for ensuring the approximation of the gas flow and the gas partial pressure of the vortex channel inside and outside the barrel-shaped sample. Thereby avoiding additional turbulence due to the pressure difference between the fluid in the inner channel and the fluid in the outer channel and further stabilizing the fluid.
Technical proposal
A vortex auxiliary system for preparing fiber reinforced composite materials by a chemical vapor infiltration method comprises a sealing system consisting of an air inlet 11, a deposition chamber 8 and an air outlet; the device is characterized by also comprising an auxiliary vortex platform positioned at the upper part of the deposition chamber; the device comprises an air inlet, an auxiliary vortex platform 10, a deposition chamber 8 and an air outlet 7 from bottom to top; the auxiliary vortex platform comprises n pairs of through holes which are uniformly distributed along the circumference and are communicated with the deposition chamber 8, an inner vortex air inlet channel 1 and an outer vortex air inlet channel 2 are formed, an inner vortex channel 5 which is communicated with an air inlet is arranged in the center, and n gas path adjusting blades 3 are arranged on the periphery of the inner vortex channel 5; the outlet of the inner measuring tangent of the gas path adjusting blade 3 is matched with the inlet tangent of the inner vortex gas inlet channel 1, and the direction of the outer arc back gas flow is matched with the direction of the gas flow inlet of the outer vortex gas inlet channel 2; after the mould is assembled in sequence from bottom to top, gas enters from the gas inlet, n parts of fluid are divided at the auxiliary vortex platform 10 and respectively flow into the inner vortex and the outer vortex gas inlet channels to form two vortices, and the inner vortex and the outer vortex respectively carry out the osmotic deposition of the fluid on the inner surface and the outer surface of a deposited product.
The through holes communicated with the deposition chamber 8 by the gas path adjusting blade 3 meet the following conditions:
R 2 ＝15.6r 2
wherein: r is the radius of the inner vortex air inlet channel and the radius of the outer vortex air inlet channel, R is the radius of the inner cylinder hole of the deposited product, and d 0 For the width of the outer vortex channel d 1 For the width of the outlet of the internal and external vortex channels, d 2 The width of the inner vortex channel is i is the length of the vortex tail wing in the adjusting blade, and n is the total number of the vortex channels.
A method for chemical vapor infiltration densification of a fiber reinforced composite material by using a vortex auxiliary system for preparing the fiber reinforced composite material by using the chemical vapor infiltration method is characterized by comprising the following steps:
step 1: preparing a hollow cylindrical fiber preform;
step 2: assembling the vortex auxiliary system according to the sequence of the air inlet, the vortex auxiliary platform, the deposition chamber and the air outlet, fixing the prefabricated body in the system, then placing the prefabricated body in a high-temperature vacuum furnace, and performing preliminary chemical vapor infiltration densification until the relative density is close to 0.5-0.6 g/cm 3 ；
Step 3: removing fiber burrs protruding from the surface of the preform, cleaning and drying;
step 4: the prefabricated body is put into a vortex auxiliary system again and then is put into a high-temperature vacuum furnace for chemical vapor infiltration densification until the relative density reaches 1.60-1.70 g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Accelerating the diffusion of the air flow in the preform sample by utilizing the inner and outer vortex formed on the inner and outer sides of the hollow cylindrical preform;
step 5: cleaning the hole sealing on the surface layer of the sample by using a mechanical method, and carrying out fine surface grinding to provide more diffusion channels for gas;
step 6: the treated preform sample is put into a vortex auxiliary system again and then is put into a high-temperature vacuum furnace for chemical vapor infiltration densification until the relative density reaches 1.80-1.90 g/cm 3 The above.
The inner diameter of the preform is 6 mm-8 mm, and the outer diameter of the preform is 40 mm-48 mm.
When the step 2, the step 4 and the step 6 are performed with chemical vapor infiltration densification, the process parameters are deposition temperature 1050-1150, atmosphere pressure 3500-5000 Pa, methane: 20ml/min, 200-300 ml/min of hydrogen, 10-16 ml/min of carrier gas hydrogen, 450-600 ml/min of argon, deposition for 50-60 h, natural cooling and removing the preform from the stoneTaking out from the ink mould to obtain the ink with the density of 0.5-0.6 g/cm 3 C/Cx-SiCy composite material of (C).
The molar mass ratio of hydrogen to MTS is 10:1.
The deposition process is repeated a plurality of times to satisfy the density as a principle.
In the step 3, the outer surface of the composite material cylinder is ground by 1 mm-2.5 mm, and the inner surface is ground by 1.5-2.5 mm.
The outer surface is ground by 0.5mm and the inner surface is ground by 1mm in the step 5.
Soaking the ground composite material in alcohol, performing ultrasonic cleaning to remove surface impurities, and drying.
Advantageous effects
According to the vortex auxiliary system and the preparation method for preparing the fiber reinforced composite material by the chemical vapor infiltration method, when the ceramic matrix composite material is prepared by using a conventional CVI mode, an inner layer vortex and an outer layer vortex are constructed through the vortex auxiliary system, so that the gas has an initial speed of moving towards the inside of the fiber preform when passing through the surface of the fiber preform. So that the gas diffusion dynamics during densification have a vortex flow diffusion dynamics. Meanwhile, the mode of removing the outer hole sealing layer by mechanical processing is adopted in addition to the vortex auxiliary deposition mode, so that the compactness and the density uniformity of the composite material prepared by CVI are improved, the diffusion depth of about 10mm can be realized, the preparation of the large-size ceramic matrix composite material is realized, and the relative density is more than 90%.
The invention has the beneficial effects that: a system for vortex-assisted chemical vapor infiltration co-deposition of densified fiber reinforced composites increases the kinetic energy of gas diffusion, so that the deposition system increases the depth of gas flow infiltration, and thicker hollow cylinder samples (greater than 10 mm) can be prepared. And as a core index of the CVI composite material, the density of the material is also improved.
Due to the design of the auxiliary vortex platform of the vortex auxiliary system (see fig. 3) in the mould, after the gas flow enters the auxiliary vortex mould from the channel, the reaction fluid is divided into two parts, one part enters the inner vortex channel and the other part enters the outer vortex channel. And due to the channel geometryAnd (3) the design is that after the gas passes through the gas groove in the platform, the gas is converged in the constant temperature reaction chamber, and fluid with vortex characteristics is respectively formed inside and outside the hollow cylindrical prefabricated body. As the vortex has the characteristics of uniform mixing and diffusion acceleration, compared with the traditional carbon-rich co-deposition C/Cx-SiCy composite material preparation technology, the system for assisting the CVI deposition by the vortex can lead the density of thicker ceramic matrix composite material (with the thickness of 10 mm-15 mm) to reach 1.80g/cm 3 ～1.90g/cm 3 (see example 1 and example 2). The average density of the hollow cylindrical sample (thickness is 10 mm) prepared by the traditional CVI laminar flow mould without using the system is only 1.35g/cm 3 (see example 3). Compared with the sample deposited in the traditional way, the material prepared by the CVI deposition way assisted by vortex has smaller internal pores, higher density and larger penetration depth.
As is apparent from fig. 8, the sample prepared by the vortex-assisted CVI method is very densely deposited at the crossing portion of the fiber bundles, and the pores of the material prepared by the conventional method have a "hole sealing" phenomenon between the fiber bundles. The hole sealing phenomenon is caused by insufficient diffusion power caused by the fact that the reaction gas source is perpendicular to the concentration diffusion direction, so that the reaction gas source is accumulated on the outer side of the prefabricated body to perform reaction accumulation, a diffusion channel which is deep and inward in the prefabricated body is blocked, and larger closed pores are formed. After the CVI mode assisted by vortex is used, the reaction gas source and the concentration diffusion direction are the same, so that the gas flow is easier to diffuse inwards, the reaction gas source cannot be accumulated on the surface of the prefabricated body by the 'blowing' of the vortex, and then the reaction gas source diffuses inwards, so that the 'hole sealing' part is pushed into the sample. The data for density and porosity in fig. 9 also supports the above description well. For the composite material prepared by CVI, the density is positively correlated with the mechanical property, and when the porosity is more than 3%, the lower the porosity is, the higher the material reliability is.
The density of the carbon-rich C/Cx-SiCy composite material is only greater than 1.65g/cm 3 The method has practical application value only in the case. Sample density deposited using conventional rectifying hole die was 1.41g/cm 3 The use standard is far from being met, and the too high porosity leads the pores in the material to be densely distributed, so that the requirement of the aerospace field on the material can not be metMaterial stability requirements. As can be seen from example 1, the density of the material prepared by the vortex assisted CVI deposition method is as high as 1.85g/cm 3 Far above the minimum standard, the porosity has been close to that of widely used C/C composites. Moreover, the parameters other than the size of the fiber preform are not required, and the fiber preform can be applied to the preparation of various fiber reinforced ceramic matrix composite materials.
Drawings
FIG. 1 is a flow chart of the method of the present invention
FIG. 2 is an inlet model of a vortex assisted system.
FIG. 3 is an auxiliary vortex platform of the vortex auxiliary system.
FIG. 4 is a deposition chamber of the vortex assisted system.
Fig. 5 is an air outlet of the vortex assistance system.
Fig. 6 is a hollow cylinder preform model.
FIG. 7 shows a conventional CVI deposition rectifying orifice platform
FIG. 8 is a schematic diagram of mold assembly of the vortex assisted system
FIG. 9 is a view of the direction of movement of the vortex assisted platform fluid in the horizontal direction.
FIG. 10 is an SEM image of the internal porosity of samples at various thicknesses for the preparation of carbon-rich C/Cx-SiCy composites using conventional and vortex-assisted CVI mode. a. ) The thickness of the vortex auxiliary CVI mode is 2.5 mm; b. ) The thickness of the traditional CVI mode is 2.5 mm; c. ) The thickness of the vortex auxiliary CVI mode is 5 mm; d. ) The thickness of the traditional CVI mode is 5mm.
FIG. 11 is a graph of a.) density and b.) porosity for preparing carbon-rich C/Cx-SiCy composites using different CVI modes
Reference numerals illustrate: 1. an inner vortex air intake passage. 2. An outer vortex air intake passage. 3. And the air path is used for adjusting the blade. 4. An outer vortex channel. 5. An inner vortex passage. 6. The preform fits into the space.
Detailed Description
The invention will now be further described with reference to examples, figures:
the technical scheme of the invention is as follows: co-deposition of C/Cx-SiCy composite by using the vortex assistance system of FIGS. 1-6When the relative density of the preform is 5-20%, the surface of the preform is subjected to fine deburring treatment. The vortex auxiliary system can increase the diffusion kinetic energy of the fluid to enable the fluid to permeate into deeper pores of the preform, thereby achieving the purpose of densifying thicker samples until the density of the samples reaches 1.85g/cm 3 ～1.90g/cm 3 . Examples 1, 2 are examples of vortex assisted CVI mode preparation using the present invention. Example 3 is a counter example of a conventional rectification orifice platform (see fig. 7) was used.
The technical scheme of the invention is as follows: a vortex auxiliary system for chemical vapor infiltration densification of fiber reinforced composite materials comprises an air inlet, an auxiliary vortex platform, a deposition chamber and an air outlet. The device comprises an air inlet, an auxiliary vortex platform 10, a deposition chamber 8 and an air outlet 7 from bottom to top; the auxiliary vortex platform comprises three pairs of through holes which are uniformly distributed along the circumference and are communicated with the deposition chamber 8, an inner vortex air inlet channel 1 and an outer vortex air inlet channel 2 are formed, an inner vortex channel 5 which is communicated with an air inlet is arranged in the center, and three air path adjusting blades 3 are arranged on the periphery of the inner vortex channel 5; the outlet of the inner measuring tangent of the gas path adjusting blade 3 is matched with the inlet tangent of the inner vortex gas inlet channel 1, and the direction of the outer arc back gas flow is matched with the direction of the gas flow inlet of the outer vortex gas inlet channel 2; when the mould is assembled from bottom to top in sequence, gas enters from the gas inlet, three parts of fluid inside and outside are separated at the auxiliary vortex platform 10 and respectively flow into the inner vortex and the outer vortex gas inlet channels to form two vortices, and the inner vortex and the outer vortex respectively carry out the infiltration deposition of the fluid on the inner surface and the outer surface of a deposited product.
The through holes communicated with the deposition chamber 8 by the gas path adjusting blade 3 meet the following conditions:
R 2 ＝15.6r 2
wherein: r is the radius of the inner vortex air inlet channel and the radius of the outer vortex air inlet channel, R is the radius of the inner cylinder hole of the deposited product, and d 0 For the width of the outer vortex channel d 1 For the width of the outlet of the internal and external vortex channels，d 2 And i is the length of the vortex tail fin in the adjusting blade.
The prefabricated body is arranged above the gas path adjusting blade in the auxiliary vortex platform, the inner vortex channel and the outer vortex channel are separated by the sample, the double channels of the inner vortex and the outer vortex are formed, convection is prevented from being generated in the channels, and vortex formation is influenced.
The preparation process comprises the following steps: a hollow cylindrical fiber preform having an inner diameter of 6 to 8mm and an outer diameter of 40 to 50mm was prepared.
Step one: the vortex assisted system was assembled in the order of gas inlet, vortex assisted platform, deposition chamber, gas outlet and preform samples were fixed in the system, see fig. 8.
Step two: and assembling the mould according to the sequence of the air inlet, the auxiliary vortex platform, the deposition chamber and the air outlet, putting the prefabricated body into the mould, and placing the prefabricated body into a high-temperature vacuum furnace. The preform is deposited according to the following process parameters: deposition temperature is 1050-1150, atmosphere pressure is 3500-5000 Pa, methane: 20ml/min, 200-300 ml/min of hydrogen, 10-16 ml/min of carrier gas hydrogen and 450-600 ml/min of argon, wherein the molar mass ratio of hydrogen to MTS is 10:1. depositing for 50-60 h, naturally cooling, and repeating the deposition process for 2 times. Taking out the prefabricated body from the graphite mould to obtain 0.5-0.6 g/cm 3 And (3) performing primary chemical vapor infiltration densification on the C/Cx-SiCy composite material until the relative density is close to 5% -20%.
Step three: removing fiber burrs protruding from the surface of the preform, cleaning and drying: grinding the outer surface of the composite material cylinder by 1 mm-2.5 mm, and grinding the inner surface by 1.5-2.5 mm. Soaking the ground composite material in alcohol, performing ultrasonic cleaning for 15min to remove surface impurities, and drying in a 70 ℃ oven for 10h.
Step four: and (3) putting the preform sample into an eddy current auxiliary system again for chemical vapor infiltration densification, and repeating the process of the step (2) for the composite material to carry out densification treatment on the C/Cx-SiCy composite material for 5-6 times. Until the sample density reaches 1.60-1.70 g/cm3.
Namely, the relative density reaches 60 to 80 percent. The diffusion of the air flow inside the preform sample is accelerated by the inner and outer vortices formed at both inner and outer sides of the hollow cylindrical preform.
Step five: and cleaning the hole sealing on the surface layer of the sample by using a mechanical method, and providing more diffusion channels for gas. The outer surface was ground 0.5mm and the inner surface was ground 1mm. Soaking the ground composite material in alcohol, performing ultrasonic cleaning for 15min to remove surface impurities, and drying in a 70 ℃ oven for 10h.
Step 6: the densification of the C/Cx-SiCy composite material was performed 8 times by repeating the procedure described in step 2. The density of the final sample reaches 1.80-1.90 g/cm 3 . Until the relative density reaches more than 90 percent.
Example 1. The vortex assisted CVI codeposits densification of the carbon-rich C/Cx-SiCy composite.
Step 1: A2.5D needled carbon felt (density 0.41g/cm 3) preform was prepared as a hollow cylinder having an outer diameter of 42mm, an inner diameter of 18mm and a height of 70 mm.
Step 2: and assembling the mould according to the sequence of the air inlet, the auxiliary vortex platform, the deposition chamber and the air outlet, putting the prefabricated body into the mould, and placing the prefabricated body into a high-temperature vacuum furnace. The preform is deposited according to the following process parameters: deposition temperature 1100 ℃, atmosphere pressure 5000Pa, methane: 20ml/min, 200ml/min of hydrogen, 16ml/min of carrier gas hydrogen, 600ml/min of argon and 10 of molar mass ratio of hydrogen to MTS: 1. depositing for 50h, naturally cooling, and repeating for 2 times. The preform was removed from the graphite mold to give 0.58g/cm 3 C/Cx-SiCy composite material of (C).
Step 3: the outer surface of the composite cylinder was ground to 1mm and the inner surface was ground to 1mm. Soaking the ground composite material in alcohol, performing ultrasonic cleaning for 15min to remove surface impurities, and drying in a 70 ℃ oven for 10h.
Step 4: the densification of the C/Cx-SiCy composite material was performed 4 times by repeating the procedure described in step 2. The final sample density reached 1.60g/cm3.
Step 5: the outer surface of the composite cylinder was ground 0.5mm and the inner surface was ground 1mm. Soaking the ground composite material in alcohol, performing ultrasonic cleaning for 15min to remove surface impurities, and drying in a 70 ℃ oven for 10h.
Step 6: the densification of the C/Cx-SiCy composite material was performed 8 times by repeating the procedure described in step 2. The final sample density reached 1.85g/cm3.
Example 2. Vortex assisted CVI codeposits densification of silicon-rich C/Cx-SiCy composites.
Step 1: A2.5D needled carbon felt (density 0.41g/cm 3) preform was prepared as a hollow cylinder with an outer diameter of 45mm, an inner diameter of 6mm and a height of 70 mm.
Step 2: and assembling the mould according to the sequence of the air inlet, the auxiliary vortex platform, the deposition chamber and the air outlet, putting the prefabricated body into the mould, and placing the prefabricated body into a high-temperature vacuum furnace. The preform is deposited according to the following process parameters: deposition temperature 1150 ℃, atmosphere pressure 3500Pa, methane: 20ml/min, 300ml/min of hydrogen, 10ml/min of carrier gas hydrogen, 450ml/min of argon and 10 of molar mass ratio of hydrogen to MTS: 1. depositing for 60h, naturally cooling, and repeating for 2 times. The preform was removed from the graphite mold to give a C/Cx-SiCy composite of 0.45g/cm 3.
Step 3: grinding the outer surface of the composite material cylinder by 1 mm-2.5 mm, and grinding the inner surface by 1.5 mm-2.5 mm. Soaking the ground composite material in alcohol, performing ultrasonic cleaning for 15min to remove surface impurities, and drying in a 70 ℃ oven for 10h.
Step 4: the densification of the C/Cx-SiCy composite material was performed 5 times by repeating the procedure described in step 2. The final density of the sample reached 1.70g/cm3.
Step 5: the outer surface of the composite cylinder was ground 0.5mm and the inner surface was ground 1mm. Soaking the ground composite material in alcohol, performing ultrasonic cleaning for 15min to remove surface impurities, and drying in a 70 ℃ oven for 10h.
Step 6: the densification of the C/Cx-SiCy composite material was performed 8 times by repeating the procedure described in step 2. The final sample density reached 1.90g/cm3.
Example 3. And preparing the cylindrical codeposition carbon-rich C/Cx-SiCy composite material by adopting a traditional CVI mode.
Step 1: A2.5D needled carbon felt (density 0.41g/cm 3) preform was prepared as a hollow cylinder with an outer diameter of 40mm, an inner diameter of 18mm and a height of 70 mm.
Step 2: and assembling the mould according to the sequence of the gas inlet, the deposition chamber and the gas outlet of the traditional CVI rectifying hole deposition platform, and placing the prefabricated body in the deposition chamber and placing the prefabricated body in a high-temperature vacuum furnace. The preform is deposited according to the following process parameters: deposition temperature 1100 ℃, atmosphere pressure 5000Pa, methane: 20ml/min, 200ml/min of hydrogen, 16ml/min of carrier gas hydrogen, 600ml/min of argon and 10 of molar mass ratio of hydrogen to MTS: 1. and depositing for 52h, naturally cooling, and repeating for 2 times. The preform was removed from the graphite mold to give 0.49g/cm 3 C/Cx-SiCy composite material of (C).
Step 3: the outer surface of the composite cylinder was ground to 1mm and the inner surface was ground to 1mm. Soaking the ground composite material in alcohol, performing ultrasonic cleaning for 15min to remove surface impurities, and drying in a 70 ℃ oven for 10h.
Step 4: the densification of the C/Cx-SiCy composite material was performed 5 times by repeating the procedure described in step 2. The final sample density reached 1.01g/cm3.
Step 5: the outer surface of the composite cylinder was ground 0.5mm and the inner surface was ground 1mm. Soaking the ground composite material in alcohol, performing ultrasonic cleaning for 15min to remove surface impurities, and drying in a 70 ℃ oven for 10h.
Step 6: the densification of the C/Cx-SiCy composite material was performed 8 times by repeating the procedure described in step 2. The final sample density reached 1.20g/cm3.
Claims (9)
1. A vortex auxiliary system for preparing fiber reinforced composite materials by a chemical vapor infiltration method comprises a sealing system consisting of an air inlet (11), a deposition chamber (8) and an air outlet; the device is characterized by also comprising an auxiliary vortex platform positioned at the upper part of the deposition chamber; the device comprises an air inlet, an auxiliary vortex platform (10), a deposition chamber (8) and an air outlet (7) from bottom to top; the auxiliary vortex platform comprises n pairs of through holes which are uniformly distributed along the circumference and are communicated with the deposition chamber (8), an inner vortex air inlet channel (1) and an outer vortex air inlet channel (2) are formed, an inner vortex channel (5) which is communicated with the air inlet is arranged in the center, and n gas path adjusting blades (3) are arranged on the periphery of the inner vortex channel (5); the inner tangential line outlet of the air path adjusting blade (3) is matched with the inlet tangential line of the inner vortex air inlet channel (1), and the outer arc back air flow direction is matched with the air flow inlet direction of the outer vortex air inlet channel (2); after the mould is assembled in sequence from bottom to top, gas enters from the gas inlet, n parts of fluid are separated at the auxiliary vortex platform (10) and respectively flow into the inner vortex and the outer vortex gas inlet channels to form two vortices, and the inner vortex and the outer vortex respectively carry out fluid infiltration deposition on the inner surface and the outer surface of a deposited product;
the through holes communicated with the deposition chamber (8) of the gas path adjusting blade (3) meet the following conditions:
R 2 ＝15.6r 2
d 0 ＝0.75r,d 1 ＝1.7r,d 2 ＝d 0 ,
wherein: r is the radius of the inner vortex air inlet channel and the radius of the outer vortex air inlet channel, R is the radius of the inner cylinder hole of the deposited product, and d 0 For the width of the outer vortex channel d 1 For the width of the outlet of the internal and external vortex channels, d 2 For the width of the inner vortex channel,
i is the length of the vortex tail wing in the adjusting blade, and n is the total number of vortex channels.
2. A method for chemical vapor infiltration densification of a fiber reinforced composite material using the vortex assisted system for chemical vapor infiltration of a fiber reinforced composite material of claim 1, characterized by the steps of:
step 1: preparing a hollow cylindrical fiber preform;
step 2: assembling the vortex auxiliary system according to the sequence of the air inlet, the vortex auxiliary platform, the deposition chamber and the air outlet, fixing the prefabricated body in the system, then placing the prefabricated body in a high-temperature vacuum furnace, and performing preliminary chemical vapor infiltration densification until the relative density is close to 0.5-0.6 g/cm 3 ；
Step 3: removing fiber burrs protruding from the surface of the preform, cleaning and drying;
step 4: after the prefabricated body is re-placed into the vortex auxiliary systemPlacing the mixture in a high-temperature vacuum furnace for chemical vapor infiltration densification until the relative density reaches 1.60-1.70 g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Accelerating the diffusion of the air flow in the preform sample by utilizing the inner and outer vortex formed on the inner and outer sides of the hollow cylindrical preform;
step 5: cleaning the hole sealing on the surface layer of the sample by using a mechanical method, and carrying out fine surface grinding to provide more diffusion channels for gas;
step 6: the treated preform sample is put into a vortex auxiliary system again and then is put into a high-temperature vacuum furnace for chemical vapor infiltration densification until the relative density reaches 1.80-1.90 g/cm 3 The above.
3. The method according to claim 2, characterized in that: the inner diameter of the preform is 6 mm-8 mm, and the outer diameter of the preform is 40 mm-48 mm.
4. The method according to claim 2, characterized in that: when the step 2, the step 4 and the step 6 are performed with chemical vapor infiltration densification, the process parameters are deposition temperature 1050-1150, atmosphere pressure 3500-5000 Pa, methane: 20ml/min, 200-300 ml/min of hydrogen, 10-16 ml/min of carrier gas hydrogen, 450-600 ml/min of argon, deposition for 50-60 h, natural cooling, taking out the preform from the graphite die to obtain 0.5-0.6 g/cm 3 C/Cx-SiCy composite material of (C).
5. The method according to claim 4, wherein: the molar mass ratio of hydrogen to MTS is 10:1.
6. The method according to claim 4, wherein: the deposition process is repeated a plurality of times to satisfy the density as a principle.
7. The method according to claim 2, characterized in that: in the step 3, the outer surface of the composite material cylinder is ground by 1 mm-2.5 mm, and the inner surface is ground by 1.5-2.5 mm.
8. The method according to claim 2, characterized in that: the outer surface is ground by 0.5mm and the inner surface is ground by 1mm in the step 5.
9. The method according to claim 7 or 8, characterized in that: soaking the ground composite material in alcohol, performing ultrasonic cleaning to remove surface impurities, and drying.
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