CN115193654B - Continuous production process for impregnation-curing of fiber reinforced ceramic matrix composite - Google Patents

Continuous production process for impregnation-curing of fiber reinforced ceramic matrix composite Download PDF

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Publication number
CN115193654B
CN115193654B CN202210809202.5A CN202210809202A CN115193654B CN 115193654 B CN115193654 B CN 115193654B CN 202210809202 A CN202210809202 A CN 202210809202A CN 115193654 B CN115193654 B CN 115193654B
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area
sealing door
dipping
curing
chamber
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CN115193654A (en
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陈思安
王为得
郭蕾
马青松
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National University of Defense Technology
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National University of Defense Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C9/00—Apparatus or plant for applying liquid or other fluent material to surfaces by means not covered by any preceding group, or in which the means of applying the liquid or other fluent material is not important
    • B05C9/08—Apparatus or plant for applying liquid or other fluent material to surfaces by means not covered by any preceding group, or in which the means of applying the liquid or other fluent material is not important for applying liquid or other fluent material and performing an auxiliary operation
    • B05C9/14—Apparatus or plant for applying liquid or other fluent material to surfaces by means not covered by any preceding group, or in which the means of applying the liquid or other fluent material is not important for applying liquid or other fluent material and performing an auxiliary operation the auxiliary operation involving heating or cooling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C13/00—Means for manipulating or holding work, e.g. for separate articles
    • B05C13/02—Means for manipulating or holding work, e.g. for separate articles for particular articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C15/00—Enclosures for apparatus; Booths
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C3/00—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material
    • B05C3/02—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material
    • B05C3/09—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material for treating separate articles
    • B05C3/10—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material for treating separate articles the articles being moved through the liquid or other fluent material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
    • B05D3/0406—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases the gas being air
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
    • B05D3/0493—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases using vacuum
    • 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
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Reinforced Plastic Materials (AREA)

Abstract

The device comprises an independent and connected impregnation chamber (1) and a curing chamber (2); the top of the dipping chamber (1) is an integral space, and the lower part of the dipping chamber comprises a feeding area (6), a dipping area (7), a hanging and airing area (8) and a transferring area (9) which are respectively and sequentially connected; the transmission system (10) of the dipping chamber (1) is arranged above the inside of the dipping chamber (1) and is used for hanging materials to be dipped and solidified and conveying the materials to any one of a feeding area (6), a dipping area (7), a hanging and airing area (8) and a transferring area (9) in the dipping chamber (1); the curing chamber (2) comprises an isolation area (11), a curing area (12) and a discharging area (13) which are respectively and independently connected in sequence; a vacuum system and a protective gas supplementing system are connected with the intervals to realize vacuumizing and provide protective gas.

Description

Continuous production process for impregnation-curing of fiber reinforced ceramic matrix composite
Technical Field
The invention relates to the technical field of ceramic matrix composite manufacturing, in particular to a fiber reinforced ceramic matrix composite impregnation-curing continuous production process.
Background
The continuous fiber reinforced/toughened ceramic matrix composite material can solve the brittleness of single-phase ceramic, has higher tenacious property and impact resistance, and simultaneously has the advantages of high temperature resistance, wear resistance, oxidation resistance and the like of the ceramic.
The precursor impregnation-cracking process (Polymer infiltration and pyrolysis, PIP process for short) is one of the main processes for preparing fiber reinforced ceramic matrix composites at present. The process comprises the following steps: 1) Placing the fiber preform in a sealed container, and vacuumizing; 2) Injecting a solution or liquid precursor; 3) Impregnating for a period of time, and penetrating the precursor into the preform by capillary force; 4) Opening the sealed container, taking out the impregnated preform, airing, crosslinking and solidifying; 5) Transferring the preform to a high-temperature furnace protected by protective gas, and heating to a set temperature for cracking; 6) Cooling along with the furnace after the cracking is finished, and taking out the product; 7) Repeating the impregnation-crosslinking-pyrolysis procedure directs a dense composite material to be obtained.
At present, the impregnation equipment and the crosslinking curing equipment are independent, so that a transfer process is also arranged between the impregnation and the crosslinking curing, and the processes of vacuumizing, feeding, discharging, airing and the like between the key impregnation and curing processes need a plurality of hours, and each impregnation and curing process needs time, so that the production process of the ceramic matrix composite is a great time cost, and the potential safety hazard exists in the process of feeding and discharging the precursor for a plurality of times. Particularly for mass production, a plurality of sets of dipping and curing equipment are required, the operation space and the operation time are easy to interfere, and automation is not easy to realize.
Disclosure of Invention
The invention aims to solve the technical problem of providing a continuous production process for impregnating-curing fiber reinforced ceramic matrix composite materials, aiming at the defects in the prior art.
The technical scheme of the invention is that the fiber reinforced ceramic matrix composite material dipping-curing continuous production process uses a fiber reinforced ceramic matrix composite material dipping-curing continuous production device, and comprises a dipping chamber and a curing chamber which are respectively independent and are in sealing connection; the dipping chamber and the curing chamber are made of stainless steel or carbon steel; the top of the dipping chamber is an integral space, and the lower part of the dipping chamber comprises a feeding area, a dipping area, a hanging and airing area and a transferring area which are respectively and sequentially connected; the impregnation chamber further comprises a transmission system; the transmission system is arranged above the inside of the dipping chamber and is used for hanging materials to be dipped and solidified and conveying the materials to any one of a feeding area, a dipping area, a hanging and airing area and a transferring area in the dipping chamber.
Furthermore, the fiber reinforced ceramic matrix composite material dipping-curing continuous production device also comprises a vacuum system, a liquid supplementing system and a protective gas supplementing system; the vacuum system is respectively communicated with a feeding zone, an impregnation zone and a transfer zone of the impregnation chamber; the liquid supplementing system is communicated with the dipping area of the dipping chamber and is used for supplementing dipping liquid to the dipping area; the protective gas supplementing system is communicated with the feeding area, the dipping area, the transferring area and the curing chamber of the dipping chamber and is used for supplementing protective gas into the curing chamber; the transmission system comprises a lifting device and a hook, wherein the lifting device is connected with the top of the dipping chamber and is used for enabling materials to be dipped and cured and loading containers thereof to be at different heights in the dipping region; the top of the hook is connected with the lifting device, and the lower part of the hook is used for hooking the material to be impregnated-cured and the loading container thereof.
Further, the feeding zone is provided with a second sealing door and a first sealing door on one side of the top and the wall of the dipping chamber respectively; the first sealing door is used for enabling materials to be impregnated and solidified to enter the feeding area and sealing the impregnation chamber and the feeding area; the second sealing door is used for maintaining the vacuum state of the impregnation zone during the feeding process to the feeding zone; the top of the hanging and airing area is a slope gradually rising from the position close to the dipping area to the position close to the transferring area so as to be beneficial to the dipping liquid in the dipped material to drop back into the dipping area; the top of the transfer area, the connection surface of the transfer area and the isolation area are respectively provided with a third sealing door and a fourth sealing door, and the third sealing door is used for keeping the vacuum of the dipping chamber in the process of transferring materials out of the dipping chamber; the fourth sealing door is used for transferring materials out of the dipping chamber and realizing sealing isolation between the dipping chamber and the curing chamber; the partition plates between the feeding area and the soaking area and the three partition plates surrounding the hanging and airing area are made of stainless steel or carbon steel.
Further, the curing chamber comprises an isolation area, a curing area and a discharging area which are respectively and independently connected in sequence; the protective gas supplementing system is communicated with the curing zone and the discharging zone; the vacuum system is communicated with the curing area and the discharging area; heating resistance wires are distributed on the inner walls of each side of the curing zone; the isolation area is connected with the transfer area of the dipping chamber; a fifth sealing door is arranged between the curing zone and the discharging zone; the discharging area is provided with a sixth sealing door on the wall of the curing chamber; the fourth sealing door, the fifth sealing door and the sixth sealing door are made of stainless steel or common carbon steel, and are matched with a silica gel or fluorine gel sealing ring on the periphery to achieve sealing effect, and the closing and the opening are controlled by an electromechanical device; the junction gate between isolation district and the solidification district is the thermal insulation material in area space, and its switch is forward induction type resilience switch, and is automatic open when sensing the material and be close, and the back automatic shutdown is left to the material.
Further, the transmission system further comprises a rail and an electric driving control device; the track is arranged at the top of the dipping chamber and provides a horizontal running channel for the lifting device; the electric driving control device is connected with the track and the lifting device, provides driving force for the lifting device to move on the track and controls the descending height of the lifting device; the track of the transmission system is in a shape like a Chinese character 'kou' in the dipping chamber, so that after the material is unloaded in the transferring area, the empty hooks return to the upper part of the feeding area.
Furthermore, the fiber reinforced ceramic matrix composite material dipping-curing continuous production device also comprises a vacuum gauge and a liquid level gauge; the vacuum gauge is arranged above the dipping chamber; the liquid level meter is arranged in the impregnation zone and is used for measuring the liquid level height of the impregnation zone; the material to be impregnated-solidified is loaded in a stainless steel hollowed-out material frame which is hung on a hook of the transmission system.
The invention relates to a fiber reinforced ceramic matrix composite impregnation-curing continuous production process, which specifically comprises the following steps:
1) Feeding liquid: the first sealing door, the second sealing door, the third sealing door, the fourth sealing door and the fifth sealing door of the fiber reinforced ceramic matrix composite material dipping-curing continuous production device are in a closed state, all the sections in the dipping chamber are vacuumized to-0.1 MPa through a vacuum system, and then a precursor solution or a liquid precursor is injected into the dipping section through a liquid supplementing system to serve as dipping liquid;
2) Feeding: charging the feeding area to normal pressure, opening a first sealing door, pushing the material to be impregnated-solidified or a stainless steel hollowed-out material frame filled with the material to be impregnated-solidified into the feeding area, closing the first sealing door, and vacuumizing the feeding area to-0.1 MPa;
3) First transfer: opening a second sealing door, enabling a hook of a transmission system to hang a material to be impregnated-solidified or a stainless steel hollowed-out material frame filled with the material to be impregnated-solidified, lifting and transferring the material to impregnating liquid in an impregnation area, closing the second sealing door, and vacuumizing to-0.1 MPa;
4) The dipping step comprises the following steps: vacuum dipping the material to be dipped and cured or the stainless steel hollow material frame filled with the material to be dipped and cured in dipping liquid;
5) And (3) airing: when the material to be impregnated-cured or the stainless steel hollow material frame filled with the material to be impregnated-cured moves to the interface between the impregnation area and the hanging and airing area, the transmission system lifts the material to be impregnated-cured or the stainless steel hollow material frame filled with the material to be impregnated-cured off the impregnation liquid, and hanging and airing the material in the hanging and airing area;
6) Second transfer: opening a third sealing door, hanging a material to be impregnated-cured or a stainless steel hollow material frame filled with the material to be impregnated-cured into a transfer area by a transmission system, separating a hook of the transmission system from the material to be impregnated-cured or the stainless steel hollow material frame filled with the material to be impregnated-cured, and closing the third sealing door; meanwhile, the transmission system returns to the upper part of the feeding area to continuously hook the materials to be impregnated and cured of the next batch or a stainless steel hollowed-out material frame filled with the materials to be impregnated and cured;
7) Opening a fourth sealing door, introducing protective gas into each region between the transfer region and the curing region, transferring the material to be impregnated-cured or the stainless steel hollowed-out material frame filled with the material to be impregnated-cured to the curing region, and closing the fourth sealing door;
8) Curing: curing the material to be impregnated-cured or the stainless steel hollow material frame filled with the material to be impregnated-cured in a curing zone which is heated to a set temperature in advance for 2-8 hours at 50-250 ℃;
9) Discharging: and opening a fifth sealing door, introducing protective gas into a discharging area, transferring the material to be impregnated-cured or the stainless steel hollow material frame filled with the material to be impregnated-cured out of the curing area, closing the fifth sealing door, opening the sixth sealing door to discharge, finishing discharging, and closing the sixth sealing door and the protective gas to finish the impregnation-curing process of the material to be impregnated-cured.
Further, in the step 4), the vacuum impregnation time is controlled to be 8-24 hours; in the step 5), the hanging and airing time is 2-4 hours; in the steps 6) to 9), the shielding gas is replaced by air.
Compared with the prior art, the invention has the advantages that:
1. in the continuous production process for impregnating-curing the fiber reinforced ceramic matrix composite, the impregnating equipment and the curing equipment are integrated integrally, so that the whole impregnating-curing process of the fiber reinforced ceramic matrix composite can be in a vacuum or protective gas protection state in the whole process, the continuous production process is particularly suitable for precursor solution or liquid precursor with higher self-storage stability, and the defects of large quantity of impregnating-curing equipment and low automation degree in the large-scale production process of the fiber reinforced ceramic matrix composite are overcome.
2. Compared with the existing process flow, the continuous production method for the fiber reinforced ceramic matrix composite material impregnation-curing reduces the feeding and discharging processes of the precursor, integrates and automates the impregnation-curing flow, and can improve the production efficiency of the process by 50%.
Drawings
These and/or other aspects and advantages of the present invention will become more apparent and more readily appreciated from the following detailed description of the embodiments of the invention, taken in conjunction with the accompanying drawings, wherein:
FIG. 1 is a schematic structural view of a continuous production apparatus for impregnating-curing fiber-reinforced ceramic matrix composites in accordance with an embodiment of the present invention.
Detailed Description
The present invention will be described in further detail below with reference to the drawings and detailed description for the purpose of enabling those skilled in the art to understand the invention better.
Example 1
The fiber reinforced ceramic matrix composite material impregnating-curing continuous production device has the structure shown in figure 1, and comprises an impregnating chamber 1, a curing chamber 2, a vacuum system 3, a liquid supplementing system 4 and a protective gas supplementing system 5 which are respectively independent and are in sealing connection, wherein the whole structure and the mutual connection relation are as follows:
the dipping chamber 1 and the curing chamber 2 are made of stainless steel or common carbon steel;
the top of the dipping chamber 1 is an integral space, the lower parts of the dipping chamber 1 are respectively and independently connected with a feeding area 6, a dipping area 7, a hanging and airing area 8 and a transferring area 9 in sequence, and a transmission system 10 is also arranged in the dipping chamber 1; the transmission system 10 is arranged above the inside of the dipping chamber 1 and is used for hanging materials to be dipped and cured and conveying the materials to any one of a feeding area 6, a dipping area 7, a hanging and airing area 8 and a transferring area 9 in the dipping chamber 1;
the curing chamber 2 comprises an isolation area 11, a curing area 12 and a discharging area 13 which are respectively and independently connected in sequence;
the vacuum system 3 is respectively communicated with a feeding zone 6, an impregnating zone 7, a transferring zone 9, a curing zone 12 and a discharging zone 13 of the impregnating chamber 1;
the liquid supplementing system 4 is communicated with the dipping zone 7 of the dipping chamber 1 and is used for supplementing dipping liquid to the dipping zone 7;
the protective gas supplementing system 5 is communicated with the feeding zone 6, the dipping zone 7, the transferring zone 9, the curing chamber 2 and the discharging zone 13 of the dipping chamber 1 and is used for supplementing protective gas into the curing chamber 2.
The optimal design of each part is as follows:
the transmission system 10 comprises a lifting device and a hook, wherein the lifting device is connected with the top of the dipping chamber 1 and is used for enabling materials to be dipped and cured and loading containers thereof to be positioned at different heights in the dipping area 7; the top of the hook is connected with the lifting device, and the lower part of the hook is used for hooking the material to be impregnated-cured and the loading container thereof.
The feeding zone 6 is provided with a second sealing door II and a first sealing door I on the top and one side of the wall of the dipping chamber 1 respectively; the first sealing door I is used for enabling materials to be impregnated and cured to enter the feeding area 6 and sealing the impregnating chamber 1 and the feeding area 6; the second sealing door I is used for maintaining the vacuum state of the impregnation zone 7 during the feeding process to the feeding zone 6;
the top of the hanging and airing area 8 is a slope gradually rising from the position close to the dipping area 7 to the position close to the transferring area 9 so as to be beneficial to the dipping liquid in the dipped materials to drop back into the dipping area 7;
a third sealing door III and a fourth sealing door IV are respectively arranged at the top of the transfer area 9 and the connecting surface of the transfer area 9 and the isolation area 11, and the third sealing door III is used for keeping the vacuum of the dipping chamber 1 in the process of transferring materials out of the dipping chamber 1; the fourth sealing door IV is used for transferring materials out of the dipping chamber 1 and realizing sealing isolation between the dipping chamber 1 and the curing chamber 2;
the partition plates between the feeding area 6 and the soaking area 7 and the three partition plates surrounding the hanging and airing area 8 are made of stainless steel or common carbon steel.
Heating resistance wires are distributed on the inner walls of each side of the curing zone 12;
the isolation zone 11 is connected to the transfer zone 9 of the impregnation chamber 1;
a fifth sealing door V is arranged between the curing zone 12 and the discharging zone 13;
the discharging area 13 is provided with a sixth sealing door VI on the wall of the curing chamber 2;
the peripheries of the fourth sealing door IV, the fifth sealing door V and the sixth sealing door VI are made of stainless steel or common carbon steel, and matched with a silica gel or fluorine gel sealing ring to achieve a sealing effect, and the closing and the opening are controlled by an electromechanical device;
the junction gate between isolation zone 11 and solidification district 12 is the thermal-insulated material in area space, and its switch is forward induction type rebound switch, and is automatic open when sensing the material and be close, and the back automatic shutdown is left to the material.
The transmission system 10 further comprises a track and an electric drive control device; the track is arranged at the top of the dipping chamber 1 and provides a horizontal running channel for the lifting device; the electric driving control device is connected with the track and the lifting device, provides driving force for the lifting device to move on the track and controls the descending height of the lifting device;
the track of the drive system 10 is of a square design inside the impregnation chamber 1 so that after the material has been removed in the transfer zone 9, the empty hooks return to above the feed zone 6.
The device also comprises a vacuum gauge and a liquid level gauge;
the vacuum gauge is arranged above the dipping chamber 1;
the liquid level meter is arranged in the dipping area 7 and is used for measuring the liquid level height of the dipping area 7;
the material to be impregnated-cured is loaded in a stainless steel hollowed-out material frame A, and the stainless steel hollowed-out material frame A is hung on a hook of the transmission system 10.
Example 2
A fiber-reinforced ceramic matrix composite impregnation-curing continuous production method, which uses the fiber-reinforced ceramic matrix composite impregnation-curing continuous production device of example 1, comprising the following steps:
s1, liquid inlet: injecting 50% polycarbosilane/divinylbenzene precursor solution into the impregnation zone 7;
s3, feeding: filling a flat carbon fiber preform to be impregnated-cured into a stainless steel hollow material frame A, filling air into a feeding area 6 to normal pressure, opening a first sealing door I, pushing the stainless steel hollow material frame A filled with the preform into the feeding area 6, and vacuumizing to-0.1 MPa;
s4, first transfer: and opening the second sealing door II, hanging a hook in the transmission system 10 on the stainless steel hollowed-out material frame A, lifting and transferring the hook into 50% polycarbosilane/divinylbenzene precursor solution in the dipping region 7, and closing the second sealing door II.
S5, dipping: immersing the material frame A into 50% polycarbosilane/divinylbenzene precursor solution through the transmission system 10, adjusting the speed of the transmission system 10 to control the material frame A to move forwards, and controlling the immersing time to be 8 hours generally;
s6, airing: when the material frame A moves to the airing area 8, the transmission system 10 lifts the material frame A away from the impregnating solution B, and the airing time is generally 2 hours in the airing area 8;
s7, second transfer: opening a third sealing door III, hanging a material frame A into a transfer area 9 through a transmission system 10, separating a hook from the material frame A, closing the third sealing door III, introducing inert gas (if a precursor solution or a liquid precursor curing environment has no special requirement or the curing area is communicated with the external environment) into a curing area 12 from the transfer area 9, opening a fourth sealing door IV, and transferring the material frame A to the curing area 12;
s8, curing: the curing zone 12 is heated to 250 ℃ in the air-dried gap of the workpiece, and is cured for 2 hours;
s9, discharging: after curing, the material frame A is transferred to a discharging area 13, and the material frame A is discharged after a sixth sealing door VI of the door is opened to complete the dipping-curing process.
Example 3
A fiber-reinforced ceramic matrix composite impregnation-curing continuous production method, which uses the fiber-reinforced ceramic matrix composite impregnation-curing continuous production device of example 1, comprising the following steps:
s1, liquid inlet: injecting a liquid polycarbosilane precursor solution into the impregnation zone 7;
s3, feeding: filling a stainless steel hollowed-out material frame A with a tooling special-shaped carbon fiber preform to be impregnated and solidified, filling air into a feeding area 6 to normal pressure, opening a first sealing door I, pushing the stainless steel hollowed-out material frame A with the preform into the feeding area 6, and vacuumizing to-0.1 MPa;
s4, first transfer: opening a second sealing door II, hanging a hanging hook in a transmission system 10 on a material frame A, lifting and transferring the hanging hook into liquid polycarbosilane precursor solution in an impregnation zone 7, and closing the second sealing door II;
s5, dipping: immersing the material frame A into liquid polycarbosilane precursor solution through a transmission system 10, adjusting the speed of the transmission system 10 for controlling the material frame A to move forwards, and controlling the immersion time to be 24 hours;
s6, airing, namely when the material frame A moves to the airing area 8, lifting the material frame A by the transmission system 10 to be separated from the impregnating solution B, and hanging and airing for a set time in the airing area 8, wherein the hanging and airing time is 4 hours;
s7, second rotation: opening a third sealing door III, hanging a material frame A into a transfer area 9 through a transmission system 10, enabling a hook to be separated from the material frame A, closing the third sealing door III, introducing inert gas into a curing area 12 from the transfer area 9, opening a fourth sealing door IV, and transferring the material frame A to the curing area 12;
s8, curing: the curing zone 12 is heated to 50 ℃ in the air-dried gap of the workpiece, and is cured for 8 hours;
s9, discharging: after curing is completed, inert gas is introduced into the discharging area 13, the fifth sealing door V is opened, the material frame A is transferred to the discharging area 13, the fifth sealing door V is closed, the sixth sealing door VI is opened, and then discharging is completed in the dipping-curing process.
The foregoing description of embodiments of the invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.

Claims (1)

1. The fiber reinforced ceramic matrix composite impregnation-curing continuous production process is characterized by using a fiber reinforced ceramic matrix composite impregnation-curing continuous production device, wherein the fiber reinforced ceramic matrix composite impregnation-curing continuous production device comprises an impregnation chamber (1) and a curing chamber (2) which are respectively independent and are in sealing connection;
the dipping chamber (1) and the curing chamber (2) are made of stainless steel or carbon steel;
the top of the dipping chamber (1) is an integral space, and the lower part of the dipping chamber comprises a feeding area (6), a dipping area (7), a hanging and airing area (8) and a transferring area (9) which are respectively and independently connected in sequence;
the impregnation chamber (1) further comprises a transmission system (10); the transmission system (10) is arranged above the inside of the dipping chamber (1) and is used for hanging materials to be dipped and solidified and conveying the materials to any one of a feeding area (6), a dipping area (7), a hanging and airing area (8) and a transferring area (9) in the dipping chamber (1);
the device also comprises a vacuum system (3), a liquid supplementing system (4) and a protective gas supplementing system (5);
the vacuum system (3) is respectively communicated with a feeding zone (6), an impregnation zone (7) and a transfer zone (9) of the impregnation chamber (1);
the liquid supplementing system (4) is communicated with the impregnating zone (7) of the impregnating chamber (1) and is used for supplementing impregnating liquid to the impregnating zone (7);
the protective gas supplementing system (5) is communicated with the feeding zone (6), the soaking zone (7), the transferring zone (9) and the curing chamber (2) of the soaking chamber (1) and is used for supplementing protective gas into the curing chamber (2);
the transmission system (10) comprises a lifting device and a hook, wherein the lifting device is connected with the top of the dipping chamber (1) and is used for enabling materials to be dipped and solidified and loading containers thereof to be positioned at different heights of the dipping region (7); the top of the hook is connected with the lifting device, and the lower part of the hook is used for hooking the material to be impregnated-cured and the loading container thereof;
the feeding area (6) is respectively provided with a second sealing door (II) and a first sealing door (I) on the top and one side of the wall of the dipping chamber (1); the first sealing door (I) is used for enabling materials to be impregnated and cured to enter the feeding area (6) and sealing the impregnating chamber (1) and the feeding area (6); the second sealing door (II) is used for maintaining the vacuum state of the impregnation zone (7) during the feeding process to the feeding zone (6);
the top of the hanging and airing area (8) is a slope gradually rising from the position close to the dipping area (7) to the position close to the transferring area (9), so that dipping liquid in the dipped materials can be conveniently dripped into the dipping area (7);
the top of the transfer area (9) and the connecting surface of the transfer area (9) and the isolation area (11) are respectively provided with a third sealing door (III) and a fourth sealing door (IV), and the third sealing door (III) is used for keeping the vacuum of the dipping chamber (1) in the process of transferring materials out of the dipping chamber (1); the fourth sealing door (IV) is used for transferring materials out of the dipping chamber (1) and realizing sealing isolation of the dipping chamber (1) and the curing chamber (2);
the three-side partition plates surrounding the hanging and airing area (8) are made of stainless steel or carbon steel;
the curing chamber (2) comprises an isolation area (11), a curing area (12) and a discharging area (13) which are respectively and independently connected in sequence;
the protective gas supplementing system (5) is communicated with the curing zone (12) and the discharging zone (13);
the vacuum system (3) is communicated with the curing area (12) and the discharging area (13);
heating resistance wires are distributed on the inner walls of each side of the curing zone (12);
the isolation zone (11) is connected with the transfer zone (9) of the impregnation chamber (1);
a fifth sealing door (V) is arranged between the curing zone (12) and the discharging zone (13);
the discharging area (13) is provided with a sixth sealing door (VI) on the wall of the curing chamber (2);
the fourth sealing door (IV), the fifth sealing door (V) and the sixth sealing door (VI) are made of stainless steel or carbon steel, and the peripheries of the fourth sealing door, the fifth sealing door (V) and the sixth sealing door (VI) are matched with silica gel or fluorine gel sealing rings to achieve sealing effect, and the closing and the opening are controlled by an electromechanical device;
the connecting door between the isolation area (11) and the curing area (12) is made of heat insulation material with gaps, the switch is a forward induction rebound switch, the switch is automatically opened when the materials are sensed to be close, and the switch is automatically closed after the materials leave;
the transmission system (10) further comprises a rail and an electric drive control device; the track is arranged at the top of the dipping chamber (1) and provides a horizontal running channel for the lifting device; the electric driving control device is connected with the track and the lifting device and used for providing driving force for the lifting device to move on the track and controlling the lifting device to move away from the track to descend;
the track of the transmission system (10) is in a shape of a Chinese character 'kou' inside the dipping chamber (1) so that an empty hook returns to the upper part of the feeding area (6) after the material is detached in the transferring area (9);
the device also comprises a vacuum gauge and a liquid level gauge;
the vacuum gauge is arranged above the dipping chamber (1);
the liquid level meter is arranged in the dipping area (7) and is used for measuring the liquid level height of the dipping area (7);
the material to be impregnated-solidified is loaded in a stainless steel hollowed-out material frame (A), and the stainless steel hollowed-out material frame (A) is hung on a hook of the transmission system (10);
the method comprises the following steps:
1) Feeding liquid: the first sealing door (I), the second sealing door (II), the third sealing door (III), the fourth sealing door (IV) and the fifth sealing door (VI) of the fiber reinforced ceramic matrix composite material dipping-curing continuous production device are in a closed state, all the sections in the dipping chamber (1) are vacuumized to-0.1 MPa through a vacuum system (3), and then a precursor solution or a liquid precursor is injected into the dipping region (7) through a liquid supplementing system (4) to serve as dipping liquid (B);
2) Feeding: charging the feeding area (6) to normal pressure, opening a first sealing door (I), pushing a material to be impregnated-solidified or a stainless steel hollowed-out material frame (A) filled with the material to be impregnated-solidified into the feeding area (6), closing the first sealing door (I), and vacuumizing the feeding area (6) to-0.1 MPa;
3) First transfer: opening a second sealing door (II), enabling a hook of a transmission system (10) to hang a material to be impregnated-solidified or a stainless steel hollowed-out material frame (A) filled with the material to be impregnated-solidified, lifting and transferring the material to impregnating liquid (B) in an impregnating area (7), closing the second sealing door (II), and vacuumizing to-0.1 MPa;
4) The dipping step comprises the following steps: vacuum impregnating the material to be impregnated-cured or the stainless steel hollow material frame (A) filled with the material to be impregnated-cured in the impregnating solution (B);
5) And (3) airing: when the material to be impregnated-cured or the stainless steel hollowed-out material frame (A) filled with the material to be impregnated-cured moves to the interface between the impregnating area (7) and the hanging and airing area (8), the transmission system (10) lifts the material to be impregnated-cured or the stainless steel hollowed-out material frame (A) filled with the material to be impregnated-cured out of the impregnating solution (B), and hangs and dries in the hanging and airing area (8);
6) Second transfer: opening a third sealing door (III), hanging a material to be impregnated-cured or a stainless steel hollowed-out material frame (A) filled with the material to be impregnated-cured into a transfer area (9) by a transmission system (10), separating a hook of the transmission system (10) from the material to be impregnated-cured or the stainless steel hollowed-out material frame (A) filled with the material to be impregnated-cured, and closing the third sealing door (III); simultaneously, the transmission system (10) returns to the upper part of the feeding area (6) to continuously hook the material to be impregnated-cured of the next batch or the stainless steel hollowed-out material frame (A) filled with the material to be impregnated-cured;
7) Opening a fourth sealing door (IV), introducing protective gas into each region between the transfer region (9) and the curing region (12), transferring the material to be impregnated-cured or the stainless steel hollowed-out material frame (A) filled with the material to be impregnated-cured to the curing region (12), and closing the fourth sealing door (IV);
8) Curing: curing the material to be impregnated-cured or a stainless steel hollowed-out material frame (A) filled with the material to be impregnated-cured in a curing zone (12) which is heated to a set temperature in advance for 2-8 hours at 50-250 ℃;
9) Discharging: opening a fifth sealing door (V), leading in protective gas to a discharging area (13), transferring a material to be impregnated-cured or a stainless steel hollowed-out material frame (A) filled with the material to be impregnated-cured out of a curing area (12), closing the fifth sealing door (V), opening a sixth sealing door (VI) to discharge, finishing discharging, closing the sixth sealing door (VI) and the protective gas, and finishing the impregnation-curing process of the material to be impregnated-cured;
in the step 4), the vacuum impregnation time is controlled to be 8-24 hours;
in the step 5), the hanging and airing time is 2-4 hours;
in the steps 6) to 9), the shielding gas is replaced by air.
CN202210809202.5A 2022-07-11 2022-07-11 Continuous production process for impregnation-curing of fiber reinforced ceramic matrix composite Active CN115193654B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6483081B1 (en) * 2000-11-27 2002-11-19 Novellus Systems, Inc. In-line cure furnace and method for using the same
CN101157417A (en) * 2006-10-02 2008-04-09 袁海容 Automatic impregnating production-line equipment
CN109261457A (en) * 2018-10-17 2019-01-25 张家港市双成电工设备有限公司 A kind of environmental protection impregnating equipment and its dipping method
CN113369099A (en) * 2020-03-09 2021-09-10 株洲弗拉德科技有限公司 Tunnel type vacuum continuous impregnation production system
CN114042613A (en) * 2021-11-29 2022-02-15 浙江科力厌氧胶有限公司 Colloid curing device and curing process thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060172076A1 (en) * 2002-08-30 2006-08-03 Lord Corporation Autodeposition metal dip coating process

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6483081B1 (en) * 2000-11-27 2002-11-19 Novellus Systems, Inc. In-line cure furnace and method for using the same
CN101157417A (en) * 2006-10-02 2008-04-09 袁海容 Automatic impregnating production-line equipment
CN109261457A (en) * 2018-10-17 2019-01-25 张家港市双成电工设备有限公司 A kind of environmental protection impregnating equipment and its dipping method
CN113369099A (en) * 2020-03-09 2021-09-10 株洲弗拉德科技有限公司 Tunnel type vacuum continuous impregnation production system
CN114042613A (en) * 2021-11-29 2022-02-15 浙江科力厌氧胶有限公司 Colloid curing device and curing process thereof

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