CN115193654A - Impregnation-curing continuous production device and method for fiber-reinforced ceramic matrix composite - Google Patents
Impregnation-curing continuous production device and method for fiber-reinforced ceramic matrix composite Download PDFInfo
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- CN115193654A CN115193654A CN202210809202.5A CN202210809202A CN115193654A CN 115193654 A CN115193654 A CN 115193654A CN 202210809202 A CN202210809202 A CN 202210809202A CN 115193654 A CN115193654 A CN 115193654A
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- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 239000011159 matrix material Substances 0.000 title claims abstract description 32
- 239000011226 reinforced ceramic Substances 0.000 title claims abstract description 32
- 238000010924 continuous production Methods 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims description 36
- 239000000463 material Substances 0.000 claims abstract description 128
- 238000005470 impregnation Methods 0.000 claims abstract description 114
- 238000012546 transfer Methods 0.000 claims abstract description 49
- 230000005540 biological transmission Effects 0.000 claims abstract description 42
- 239000000835 fiber Substances 0.000 claims abstract description 32
- 238000007599 discharging Methods 0.000 claims abstract description 31
- 238000007598 dipping method Methods 0.000 claims abstract description 30
- 230000001681 protective effect Effects 0.000 claims abstract description 23
- 238000002955 isolation Methods 0.000 claims abstract description 16
- 238000007711 solidification Methods 0.000 claims abstract description 6
- 230000008023 solidification Effects 0.000 claims abstract description 3
- 238000007789 sealing Methods 0.000 claims description 107
- 239000010935 stainless steel Substances 0.000 claims description 46
- 229910001220 stainless steel Inorganic materials 0.000 claims description 46
- 239000007788 liquid Substances 0.000 claims description 37
- 239000011796 hollow space material Substances 0.000 claims description 22
- 239000002243 precursor Substances 0.000 claims description 14
- 230000001502 supplementing effect Effects 0.000 claims description 13
- 229910000975 Carbon steel Inorganic materials 0.000 claims description 12
- 239000010962 carbon steel Substances 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 7
- 238000005192 partition Methods 0.000 claims description 6
- 239000012705 liquid precursor Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000013459 approach Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 239000011737 fluorine Substances 0.000 claims description 3
- 239000000499 gel Substances 0.000 claims description 3
- 230000006698 induction Effects 0.000 claims description 3
- 239000011810 insulating material Substances 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims description 3
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- 238000013036 cure process Methods 0.000 claims 2
- 238000005086 pumping Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 13
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 6
- 229920003257 polycarbosilane Polymers 0.000 description 6
- 238000005336 cracking Methods 0.000 description 4
- 239000011153 ceramic matrix composite Substances 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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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
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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
- 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
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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
- 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
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- 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
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- 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
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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
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
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- Reinforced Plastic Materials (AREA)
Abstract
A continuous production device for impregnation-solidification of a fiber reinforced ceramic matrix composite is provided, which comprises an impregnation chamber (1) and a solidification chamber (2) which are independent and connected with each other; 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 transfer area (9) which are independent and sequentially connected; the transmission system (10) of the impregnation chamber (1) is arranged above the interior of the impregnation chamber (1) and used for suspending a material to be impregnated and cured and conveying the material to any one of a feeding area (6), an impregnation area (7), a hanging and airing area (8) and a transfer area (9) in the impregnation chamber (1); the curing chamber (2) comprises an isolation region (11), a curing region (12) and a discharging region (13) which are independent from each other and are connected in sequence; a vacuum system and a protective gas replenishing system are connected with the above sections to realize vacuum pumping and protective gas supply.
Description
Technical Field
The invention relates to the technical field of ceramic matrix composite manufacturing, in particular to a device and a method for continuous production of impregnation-curing of a fiber reinforced ceramic matrix composite.
Background
The continuous fiber reinforced/toughened ceramic matrix composite material can solve the brittleness of single-phase ceramics, has higher toughness and impact resistance, and has the advantages of high temperature resistance, wear resistance, oxidation resistance and the like of the ceramics.
A precursor impregnation-cracking process (PIP process for short) is one of the main processes for preparing the fiber reinforced ceramic matrix composite at present. The process comprises the following steps: 1) Placing the fiber preform in a sealed container, and vacuumizing; 2) Injecting a solution or a liquid precursor; 3) Dipping for a period of time, and allowing the precursor to permeate into the preform by capillary force; 4) Opening the sealed container, taking out the impregnated preform, airing, crosslinking and curing; 5) Transferring the prefabricated body to a high-temperature furnace protected by protective gas, heating to a set temperature, and cracking; 6) Cooling along with the furnace after the cracking is finished, and taking out the product; 7) The impregnation-crosslinking-cracking procedure was repeated to direct the production of a dense composite.
At present, impregnation equipment and crosslinking curing equipment are independent, so that a transfer process still exists between impregnation and crosslinking curing, processes such as vacuumizing, feeding and discharging, airing and the like among key impregnation and curing processes need hours, time is spent on each impregnation-curing process, the time cost is very large for the production process of the ceramic matrix composite, and potential safety hazards exist in the process of feeding and discharging liquid of a precursor for many times. Especially for large-scale production, a plurality of sets of dipping and curing equipment are needed, the operation space and time are easy to interfere, and automation is not easy to realize.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art and provides a device and a method for continuous production of impregnation-curing of a fiber reinforced ceramic matrix composite.
The invention adopts the technical scheme that the impregnation-curing continuous production device for the fiber reinforced ceramic matrix composite comprises an impregnation chamber and a curing chamber which are independent from each other and are in sealed connection; the impregnation chamber and the curing chamber are both made of stainless steel or common carbon steel; the top of the impregnation chamber is an integral space, and the lower part of the impregnation chamber comprises a feeding area, an impregnation area, a hanging and airing area and a transfer area which are independent from each other and are connected in sequence; the impregnation chamber further comprises a transmission system; the transmission system is arranged above the interior of the impregnation chamber and used for suspending a material to be impregnated and solidified and conveying the material to any one of a feeding area, an impregnation area, a hanging and airing area and a transfer area in the impregnation chamber.
Furthermore, the continuous production device for impregnation-curing of the fiber reinforced ceramic matrix composite also comprises a vacuum system, a liquid supplementing system and a protective gas supplementing system; the vacuum system is respectively communicated with the feeding area, the impregnation area and the transfer area of the impregnation chamber; the liquid supplementing system is communicated with the impregnation area of the impregnation chamber and is used for supplementing impregnation liquid to the impregnation area; the protective gas replenishing system is communicated with the feeding area, the impregnation area, the transfer area and the curing chamber of the impregnation chamber and is used for replenishing 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 impregnation chamber and is used for enabling the materials to be impregnated and solidified and the loading containers thereof to be positioned at different heights in the impregnation zone; 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 and solidified and the loading container thereof.
Furthermore, a second sealing door and a first sealing door are respectively arranged on the top of the feeding area and one side of the wall of the dipping chamber; the first sealing door is used for allowing 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 transfer area, so that dipping liquid drops in the dipped materials can fall 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 doors are used for keeping the vacuum of the impregnation chamber in the process of transferring the materials out of the impregnation chamber; the fourth sealing door is used for transferring the materials out of the impregnation chamber and realizing the sealing isolation of the impregnation chamber and the curing chamber; the partition board between the feeding area and the dipping area and the three-side partition board which encloses the hanging and airing area are made of stainless steel or common carbon steel.
Further, the curing chamber comprises an isolation region, a curing region and a discharging region which are independent from each other and are connected in sequence; the protective gas supplementing system is communicated with the curing area and the discharging area; the vacuum system is communicated with the curing area and the discharging area; heating resistance wires are distributed on the inner wall of each side of the curing area; the isolation zone is connected with the transfer zone of the impregnation chamber; a fifth sealing door is arranged between the curing area and the discharging area; a sixth sealing door is arranged on the wall of the curing chamber in the discharging area; the fourth sealing door, the fifth sealing door and the sixth sealing door are made of stainless steel or common carbon steel, the peripheries of the stainless steel or common carbon steel are matched with silica gel or fluorine gel sealing rings to achieve a sealing effect, and the fourth sealing door, the fifth sealing door and the sixth sealing door are controlled to be closed and opened through an electric mechanical device; the connecting door between the isolation area and the curing area is made of heat-insulating materials with gaps, the switch is a forward induction type rebound switch, the switch is automatically opened when the materials are induced to approach, and the switch is automatically closed after the materials leave.
Further, the transmission system also comprises a track and an electric drive 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 run on the track and controls the descending height of the lifting device; the track of the transmission system is designed in a square shape inside the impregnation chamber, so that after the materials are unloaded in the transfer zone, empty hooks return to the upper part of the feeding zone.
Furthermore, the impregnation-curing continuous production device for the fiber reinforced ceramic matrix composite material also comprises a vacuum gauge and a liquid level meter; the vacuum gauge is arranged above the impregnation chamber; the liquid level meter is arranged in the dipping area and used for measuring the liquid level height of the dipping area; the material to be impregnated and solidified is loaded in a stainless steel hollowed-out material frame, and the stainless steel hollowed-out material frame is hung on a hook of the transmission system.
The invention also provides a continuous production process for impregnating and curing the fiber reinforced ceramic matrix composite, which uses the continuous production device for impregnating and curing the fiber reinforced ceramic matrix composite, wherein when the impregnated and cured material enters the impregnation chamber through the feeding area, the impregnated and cured material is suspended by a transmission system and then sequentially impregnated and hung in the impregnation area and the hanging area, and then enters the curing chamber from the transfer area for curing; and the transmission system returns to the upper part of the feeding area after unloading the materials in the transfer area and then loads the next batch of materials to be impregnated and solidified.
Further, the impregnation-curing continuous production process of the fiber reinforced ceramic matrix composite material specifically comprises the following steps:
1) Liquid feeding: 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 impregnating-curing continuous production device are in a closed state, all sections in the impregnating chamber are vacuumized to-0.1 MPa through a vacuum system, and then precursor solution or liquid precursor is injected into the impregnating zone through a liquid supplementing system to serve as impregnating liquid;
2) Feeding: inflating the feeding area to normal pressure, opening a first sealing door, pushing the material to be impregnated and solidified or the stainless steel hollow material frame filled with the material to be impregnated and 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 the transmission system to hang the material to be impregnated and solidified or a stainless steel hollowed-out material frame filled with the material to be impregnated and solidified, hoisting and transferring the material to impregnating solution in an impregnation area, closing the second sealing door, and vacuumizing to-0.1 MPa;
4) And (3) dipping: vacuum dipping the materials to be dipped and cured or the stainless steel hollow material frame filled with the materials to be dipped and cured in dipping liquid;
5) Drying: when the materials to be impregnated and solidified or the stainless steel hollow material frame filled with the materials to be impregnated and solidified move to reach the boundary surface of the impregnation area and the hanging and airing area, the transmission system lifts the materials to be impregnated and solidified or the stainless steel hollow material frame filled with the materials to be impregnated and solidified to separate from the impregnation liquid, and the materials are hung and aired in the hanging and airing area;
6) And (3) second transfer: opening a third sealing door, hanging the materials to be impregnated and cured or the stainless steel hollow material frame filled with the materials to be impregnated and cured into a transfer area by a transmission system, separating a hook of the transmission system from the materials to be impregnated and cured or the stainless steel hollow material frame filled with the materials to be impregnated and cured, and closing the third sealing door; meanwhile, the transmission system returns to the upper part of the feeding area and continues to hook the next batch of materials to be dipped and cured or the stainless steel hollow material frame filled with the materials to be dipped and cured;
7) Opening a fourth sealing door, introducing protective gas into each area between the transfer area and the curing area, transferring the materials to be impregnated and cured or the stainless steel hollow frame filled with the materials to be impregnated and cured to the curing area, and closing the fourth sealing door;
8) And (3) curing: curing the material to be impregnated and cured or the stainless steel hollow material frame filled with the material to be impregnated and cured in a curing area which is heated to a set temperature in advance for 2 to 8 hours at the temperature of between 50 and 250 ℃;
9) Discharging: and opening the fifth sealing door to lead protective gas to be introduced into the discharging area, transferring the material to be impregnated and solidified or the stainless steel hollow material frame filled with the material to be impregnated and solidified out of the solidifying 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 impregnating and solidifying process of the material to be impregnated and solidified.
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 generally 2-4 hours; in steps 6) -9), the protective gas is replaced by air.
Compared with the prior art, the invention has the advantages that:
1. in the continuous impregnation-curing production device for the fiber reinforced ceramic matrix composite, the impregnation equipment and the curing equipment are integrated, so that the whole impregnation-curing process of the fiber reinforced ceramic matrix composite can be in a vacuum or protective gas protection state, the device is particularly suitable for precursor solution or liquid precursor with high storage stability, and the defects of large quantity of impregnation-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 prior process flow, the continuous production method for impregnating and curing the fiber reinforced ceramic matrix composite reduces the feeding and discharging processes of a precursor, integrates and automates the impregnating and curing process, and can improve the production efficiency of the process by 50 percent.
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 of which:
FIG. 1 is a schematic structural view of an apparatus for continuous infusion-cure production of a fiber reinforced ceramic matrix composite according to an embodiment of the present invention.
Detailed Description
In order that those skilled in the art will better understand the present invention, the following detailed description of the invention is provided in conjunction with the accompanying drawings and the detailed description of the invention.
Example 1
A continuous production device for impregnation-solidification of fiber reinforced ceramic matrix composite material is structurally shown in figure 1 and comprises an impregnation chamber 1 and a solidification chamber 2 which are independent from each other and are hermetically connected, and a vacuum system 3, a liquid supplementing system 4 and a protective gas supplementing system 5, wherein the whole structure and the mutual connection relation are as follows:
the impregnation chamber 1 and the curing chamber 2 are both made of stainless steel or common carbon steel;
the top of the impregnation chamber 1 is an integral space, the lower parts of the impregnation chamber 1 are respectively independent and are sequentially connected with a feeding area 6, an impregnation area 7, a hanging and airing area 8 and a transfer area 9, and a transmission system 10 is further arranged in the impregnation chamber 1; the transmission system 10 is arranged above the interior of the impregnation chamber 1 and used for suspending a material to be impregnated and solidified and conveying the material to any one of a feeding area 6, an impregnation area 7, a hanging and airing area 8 and a transfer area 9 in the impregnation chamber 1;
the curing chamber 2 comprises an isolation region 11, a curing region 12 and a discharging region 13 which are independent from each other and are connected in sequence;
the vacuum system 3 is respectively communicated with the feeding area 6, the impregnation area 7, the transfer area 9, the curing area 12 and the discharging area 13 of the impregnation chamber 1;
the liquid supplementing system 4 is communicated with the impregnation zone 7 of the impregnation chamber 1 and is used for supplementing impregnation liquid to the impregnation zone 7;
the protective gas replenishing system 5 is communicated with the feeding area 6, the impregnation area 7, the transfer area 9 of the impregnation chamber 1, the curing chamber 2 and the discharging area 13 and is used for replenishing protective gas into the curing chamber 2.
The optimized 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 impregnation chamber 1 and is used for enabling the materials to be impregnated and solidified and loading containers thereof to be positioned at different heights in the impregnation zone 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 and solidified 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 impregnation chamber 1 respectively; the first sealing door I is used for allowing materials to be impregnated and solidified to enter the feeding area 6 and sealing the impregnation 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-airing area 8 is a slope gradually rising from the position close to the dipping area 7 to the position close to the transfer area 9, so that dipping liquid drops in the dipped materials can fall 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 connection 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 impregnation chamber 1 in the process of transferring the materials out of the impregnation chamber 1; the fourth sealing door IV is used for transferring the materials out of the impregnation chamber 1 and realizing the sealing isolation of the impregnation chamber 1 and the curing chamber 2;
the partition boards between the feeding area 6 and the dipping area 7 and the partition boards on three sides which surround the hanging and airing area 8 are all made of stainless steel or common carbon steel.
Heating resistance wires are distributed on the inner wall of each side of the curing area 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;
a sixth sealing door VI is arranged on the wall of the curing chamber 2 of the discharging area 13;
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, the peripheries of the stainless steel or common carbon steel and the silica gel or fluorine gel sealing rings are matched to achieve the sealing effect, and the closing and the opening and the closing are controlled by an electric mechanical device;
the connecting door between the isolation area 11 and the curing area 12 is made of heat-insulating materials with gaps, and the switch is a forward induction type rebound switch which is automatically opened when the approach of materials is sensed and 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 steeping 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 run 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 discharged in the transfer zone 9, empty hooks are returned above the feed zone 6.
The device also comprises a vacuum gauge and a liquid level gauge;
the vacuum gauge is arranged above the impregnation 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 and 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.
Example 2
A fiber reinforced ceramic matrix composite impregnation-curing continuous production method, which utilizes the fiber reinforced ceramic matrix composite impregnation-curing continuous production device of embodiment 1, comprises the following steps:
s1, liquid feeding: injecting 50% polycarbosilane/divinylbenzene precursor solution into the impregnation zone 7;
s3, feeding: filling a flat carbon fiber preform to be impregnated and cured into the stainless steel hollow material frame A, filling air into the feeding area 6 to normal pressure, opening the 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 a second sealing door II, hanging a hook in the transmission system 10 on the stainless steel hollow material frame A, hoisting and transferring the stainless steel hollow material frame A into 50% polycarbosilane/divinylbenzene precursor solution in the impregnation zone 7, and closing the second sealing door II.
S5, dipping: the material frame A is immersed into 50% polycarbosilane/divinylbenzene precursor solution through a transmission system 10, the forward moving speed of the material frame A is controlled by the transmission system 10, and the immersion time is generally controlled to be 8 hours;
s6, airing: when the material frame A moves to the airing area 8, the transmission system 10 lifts the material frame A to be separated from the steeping liquor B, and the material frame A is hung and aired in the airing area 8 for set time, wherein the hanging and airing time is generally 2 hours;
s7, second transfer: opening a third sealing door III, hoisting the material frame A into the 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, the curing area can also be communicated with the external environment) into the transfer area 9 to the curing area 12, opening a fourth sealing door IV, and transferring the material frame A to the curing area 12;
s8, curing: the curing area 12 is heated to 250 ℃ in the drying gap of the workpiece and cured for 2 hours;
s9, discharging: after the curing is finished, the material frame A is transferred to a discharging area 13, and after a sixth sealing door VI is opened, the material is discharged to finish the dipping-curing process.
Example 3
A fiber reinforced ceramic matrix composite impregnation-curing continuous production method, which utilizes the fiber reinforced ceramic matrix composite impregnation-curing continuous production device of embodiment 1, comprises the following steps:
s1, liquid feeding: injecting liquid polycarbosilane precursor solution into the impregnation zone 7;
s3, feeding: loading a special-shaped carbon fiber preform with a tool to be dipped and cured into the stainless steel hollow material frame A, filling air into the feeding area 6 to normal pressure, opening a first sealing door I, pushing the stainless steel hollow 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 hook in the transmission system 10 on the material frame A, lifting and transferring the material frame A into the liquid polycarbosilane precursor solution in the impregnation zone 7, and closing the second sealing door II;
s5, dipping: the material frame A is immersed into the liquid polycarbosilane precursor solution through the transmission system 10, the forward moving speed of the material frame A is controlled by the transmission system 10, and the immersion time is controlled to be 24 hours;
s6, airing, namely lifting the material frame A by the transmission system 10 to separate the material frame A from the impregnation liquid B when the material frame A moves to the airing area 8, and airing for a set time in the airing area 8, wherein the airing time is 4 hours;
s7, second rotation: opening a third sealing door III, hoisting the material frame A into the transfer area 9 through the transmission system 10, separating the hook from the material frame A, closing the third sealing door III, introducing inert gas into the transfer area 9 to the curing area 12, opening a fourth sealing door IV, and transferring the material frame A to the curing area 12;
s8, curing: the curing area 12 is heated to 50 ℃ in the drying gap of the workpiece and cured for 8 hours;
s9, discharging: and after the curing is finished, introducing inert gas into the discharging area 13, opening the fifth sealing door V, transferring the material frame A to the discharging area 13, closing the fifth sealing door V, and discharging after opening the sixth sealing door VI to finish the impregnation-curing process.
While embodiments of the present invention have been described above, the above description is illustrative, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
Claims (9)
1. The continuous production device for impregnation-solidification of the fiber reinforced ceramic matrix composite is characterized by comprising an impregnation chamber (1) and a solidification chamber (2) which are independent from each other and are in sealed connection;
the impregnation chamber (1) and the curing chamber (2) are both made of stainless steel or common carbon steel;
the top of the impregnation chamber (1) is an integral space, and the lower part of the impregnation chamber comprises a feeding area (6), an impregnation area (7), a hanging and airing area (8) and a transfer area (9) which are independent and sequentially connected;
the impregnation chamber (1) further comprises a transmission system (10); the transmission system (10) is arranged above the interior of the impregnation chamber (1) and used for suspending a material to be impregnated and cured and conveying the material to any one of the feeding area (6), the impregnation area (7), the hanging and airing area (8) and the transfer area (9) in the impregnation chamber (1).
2. The apparatus for continuous infusion-cure production of fiber reinforced ceramic matrix composites according to claim 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 the feeding area (6), the impregnation area (7) and the transfer area (9) of the impregnation chamber (1);
the liquid replenishing system (4) is communicated with the impregnation zone (7) of the impregnation chamber (1) and is used for replenishing impregnation liquid to the impregnation zone (7);
the protective gas replenishing system (5) is communicated with the feeding area (6), the impregnation area (7), the transfer area (9) and the curing chamber (2) of the impregnation chamber (1) and is used for replenishing 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 impregnation chamber (1) and is used for enabling the materials to be impregnated and solidified and loading containers thereof to be positioned at different heights in the impregnation zone (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 and solidified and the loading container thereof.
3. The apparatus for continuous infusion-cure production of fiber reinforced ceramic matrix composites according to claim 2,
the feeding area (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 impregnation chamber (1) respectively; the first sealing door (I) is used for enabling materials to be impregnated and solidified to enter the feeding area (6) and sealing the impregnation 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-drying area (8) is a slope gradually rising from the position close to the impregnation area (7) to the position close to the transfer area (9), so that impregnation liquid drops in the impregnated material can fall back into the impregnation 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 connection 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 impregnation chamber (1) in the process of transferring the materials out of the impregnation chamber (1); the fourth sealing door (IV) is used for transferring the materials out of the impregnation chamber (1) and realizing the sealing isolation of the impregnation chamber (1) and the curing chamber (2);
the partition board between the feeding area (6) and the dipping area (7) and the partition boards on three sides which enclose the hanging and airing area (8) are all made of stainless steel or common carbon steel.
4. The apparatus for continuous infusion-cure production of fiber reinforced ceramic matrix composites according to claim 3,
the curing chamber (2) comprises an isolation region (11), a curing region (12) and a discharging region (13) which are independent from each other and are connected in sequence;
the protective gas replenishing system (5) is communicated with the curing area (12) and the discharging area (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 wall of each side of the curing area (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 area (12) and the discharging area (13);
a sixth sealing door (VI) is arranged on the wall of the curing chamber (2) in the discharging area (13);
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, the peripheries of the stainless steel or common carbon steel and the silica gel or fluorine gel sealing rings are matched to achieve the sealing effect, and the fourth sealing door (IV), the fifth sealing door (V) and the sixth sealing door (VI) are controlled to be closed and opened and closed through an electric mechanical device;
the connecting door between the isolation area (11) and the curing area (12) is made of heat-insulating materials with gaps, the switch is a forward induction type rebound switch, the rebound switch is automatically opened when the approach of materials is induced, and the rebound switch is automatically closed after the materials leave.
5. The apparatus for continuous infusion-cure production of fiber reinforced ceramic matrix composites according to claim 4,
the transmission system (10) further comprises a track and an electric drive control device; the track is arranged at the top of the steeping 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 run on the track and controls the lifting device to leave the running track to descend;
the track of the transmission system (10) is designed in a square shape inside the steeping chamber (1), so that after the materials are unloaded in the transfer area (9), empty hooks return to the upper part of the feeding area (6).
6. The apparatus for continuous infusion-cure production of fiber reinforced ceramic matrix composites according to claim 5,
the device also comprises a vacuum gauge and a liquid level gauge;
the vacuum gauge is arranged above the impregnation 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 materials to be impregnated and solidified are 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).
7. A continuous production process for impregnation-curing of fiber reinforced ceramic matrix composite, characterized in that it uses the continuous production device for impregnation-curing of fiber reinforced ceramic matrix composite according to any of claims 1-6, the material to be impregnated and cured enters the impregnation chamber (1) through the feeding zone (6), is suspended by the transmission system (10) in the impregnation zone (7) and the hanging-drying zone (8) in sequence for impregnation-hanging-drying treatment, and then enters the curing chamber (2) from the transfer zone (9) for curing; the transmission system (10) returns to the upper part of the feeding area (6) to mount the next batch of the material to be impregnated and solidified again after unloading the material in the transfer area (9).
8. The continuous infusion-cure process of claim 7, comprising the steps of:
1) Liquid feeding: 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 impregnating-curing continuous production device are in a closed state, all sections in the impregnating 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 impregnating zone (7) through a liquid supplementing system (4) to serve as an impregnating liquid (B);
2) Feeding: inflating the feeding area (6) to normal pressure, opening a first sealing door (I), pushing the material to be impregnated and solidified or the stainless steel hollow material frame (A) filled with the material to be impregnated and 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 the transmission system (10) to hang the material to be impregnated and solidified or a stainless steel hollowed material frame (A) filled with the material to be impregnated and solidified, lifting and transferring the material to an impregnating solution (B) in an impregnation area (7), closing the second sealing door (II), and vacuumizing to-0.1 MPa;
4) And (3) dipping: dipping the material to be dipped and cured or the stainless steel hollow material frame (A) filled with the material to be dipped and cured in the dipping solution (B) in vacuum;
5) Drying: when the materials to be impregnated and solidified or the stainless steel hollow material frame (A) filled with the materials to be impregnated and solidified move to reach the interface surface of the impregnation area (7) and the hanging and airing area (8), the transmission system (10) lifts the materials to be impregnated and solidified or the stainless steel hollow material frame (A) filled with the materials to be impregnated and solidified from the impregnation liquid (B), and the materials are hung and aired in the hanging and airing area (8);
6) And (3) second transfer: opening a third sealing door (III), hoisting the material to be impregnated and cured or the stainless steel hollowed-out material frame (A) filled with the material to be impregnated and cured into the transfer area (9) by the transmission system (10), separating a hook of the transmission system (10) from the material to be impregnated and cured or the stainless steel hollowed-out material frame (A) filled with the material to be impregnated and cured, and closing the third sealing door (III); meanwhile, the transmission system (10) returns to the upper part of the feeding area (6) to hook the next batch of materials to be impregnated and solidified or the stainless steel hollow material frame (A) filled with the materials to be impregnated and solidified continuously;
7) Opening a fourth sealing door (IV), introducing protective gas into each zone between the transfer zone (9) and the curing zone (12), transferring the material to be impregnated and cured or the stainless steel hollowed-out material frame (A) filled with the material to be impregnated and cured to the curing zone (12), and closing the fourth sealing door (IV);
8) And (3) curing: curing the material to be impregnated and cured or the stainless steel hollow material frame (A) filled with the material to be impregnated and cured in the curing area (12) which is heated to the set temperature in advance for 2 to 8 hours at the temperature of between 50 and 250 ℃;
9) Discharging: and opening the fifth sealing door (V), leading protective gas to enter the discharging area (13), transferring the materials to be impregnated and solidified or the stainless steel hollow material frame (A) filled with the materials to be impregnated and solidified out of the solidifying area (12), closing the fifth sealing door (V), opening the sixth sealing door (VI) to discharge, finishing discharging, and closing the sixth sealing door (VI) and the protective gas to finish the impregnating and solidifying process of the materials to be impregnated and solidified.
9. The continuous infusion-cure process of claim 7,
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 generally 2-4 hours;
in the steps 6) -9), the protective gas is replaced by air.
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| US6483081B1 (en) * | 2000-11-27 | 2002-11-19 | Novellus Systems, Inc. | In-line cure furnace and method for using the same |
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| US6483081B1 (en) * | 2000-11-27 | 2002-11-19 | Novellus Systems, Inc. | In-line cure furnace and method for using the same |
| US20060172076A1 (en) * | 2002-08-30 | 2006-08-03 | Lord Corporation | Autodeposition metal dip coating process |
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