CN115385709B - Method for quickly compacting carbon-carbon composite material - Google Patents
Method for quickly compacting carbon-carbon composite material Download PDFInfo
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- CN115385709B CN115385709B CN202211009937.6A CN202211009937A CN115385709B CN 115385709 B CN115385709 B CN 115385709B CN 202211009937 A CN202211009937 A CN 202211009937A CN 115385709 B CN115385709 B CN 115385709B
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- 239000011203 carbon fibre reinforced carbon Substances 0.000 title claims abstract description 79
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 239000002131 composite material Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000011347 resin Substances 0.000 claims abstract description 138
- 229920005989 resin Polymers 0.000 claims abstract description 138
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 94
- 238000005470 impregnation Methods 0.000 claims abstract description 89
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 47
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims abstract description 44
- 238000001723 curing Methods 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 235000005074 zinc chloride Nutrition 0.000 claims abstract description 22
- 239000011592 zinc chloride Substances 0.000 claims abstract description 22
- 238000002791 soaking Methods 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- WIEXMPDBTYDSQF-UHFFFAOYSA-N 1,3-bis(furan-2-yl)propan-2-one Chemical compound C=1C=COC=1CC(=O)CC1=CC=CO1 WIEXMPDBTYDSQF-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000005087 graphitization Methods 0.000 claims abstract description 12
- 238000007711 solidification Methods 0.000 claims abstract description 12
- 230000008023 solidification Effects 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 238000003763 carbonization Methods 0.000 claims abstract description 9
- 238000007598 dipping method Methods 0.000 claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 238000011049 filling Methods 0.000 claims description 12
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 10
- 239000004917 carbon fiber Substances 0.000 claims description 10
- 238000012360 testing method Methods 0.000 claims description 10
- 238000000280 densification Methods 0.000 claims description 9
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 9
- 238000005229 chemical vapour deposition Methods 0.000 claims description 8
- 125000004122 cyclic group Chemical group 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 230000000630 rising effect Effects 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 20
- 229910052799 carbon Inorganic materials 0.000 abstract description 20
- 239000000463 material Substances 0.000 description 12
- 230000006835 compression Effects 0.000 description 10
- 238000007906 compression Methods 0.000 description 10
- 239000011148 porous material Substances 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000010008 shearing Methods 0.000 description 8
- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000000149 penetrating effect Effects 0.000 description 4
- 238000001223 reverse osmosis Methods 0.000 description 4
- 239000012300 argon atmosphere Substances 0.000 description 3
- 230000003139 buffering effect Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 150000002605 large molecules Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000033764 rhythmic process Effects 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/608—Green bodies or pre-forms with well-defined density
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/616—Liquid infiltration of green bodies or pre-forms
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
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Abstract
The application discloses a method for quickly compacting a carbon-carbon composite material, which comprises the steps of carrying out heat treatment on a carbon blank to obtain a carbon-carbon porous body, soaking the carbon-carbon porous body in phosphoric acid aqueous solution, obtaining the carbon-carbon porous body subjected to interface pretreatment after the soaking is finished, placing the carbon-carbon porous body subjected to interface pretreatment in an impregnating tank of an impregnating device, vacuumizing, then sucking an impregnating agent into the impregnating tank, and carrying out pressurized impregnation, curing, carbonization and graphitization; repeating the steps of pressurized impregnation, solidification, carbonization and graphitization until a compact carbon-carbon composite material is obtained; the impregnant comprises furfuryl ketone resin, phosphoric acid and zinc chloride. The application can reduce the dipping times of the carbon-carbon composite material by 10 to 40 percent, integrally improve the mechanical property by 5 to 20 percent and prolong the service life of the resin by 50 to 100 percent.
Description
Technical Field
The application relates to a method for quickly compacting a carbon-carbon composite material, and belongs to the technical field of preparation of carbon-carbon composite materials.
Background
The carbon-carbon composite material is mainly formed into matrix carbon through chemical vapor deposition, resin impregnation, asphalt impregnation and other processes, and is combined with carbon fibers to form the high-performance composite material. The impregnation process is a process of immersing a carbon/carbon composite material blank with a resin or pitch in a pressure vessel and pressing the resin into the blank pores by high pressure to increase the blank density and material properties. The mechanical properties of the impregnated composite material are mainly related to the types of resin, the degree of crosslinking of the resin and the density of the product, and the types and the proportions of the resin curing agents influence the degree of crosslinking of the resin. The efficiency of impregnation densification is mainly related to impregnation pressure, temperature, time, resin viscosity, pore interface characteristics, which have an important influence on the efficiency of impregnation densification, and reverse osmosis.
The existing resin impregnation technology mainly adopts phosphoric acid as a curing agent, has high curing efficiency and good mechanical property, but can lead to great rise of the viscosity of the resin, influence the flow of the resin in the pores of the composite material, influence the impregnation efficiency, greatly reduce the use times of the resin and shorten the preservation period.
The phosphoric acid curing agent is adopted simply, the resin becomes very viscous immediately after phosphoric acid is added, the resin is not beneficial to flowing in the pores of the material after the viscosity of the resin is increased, and the impregnation efficiency of the resin is reduced. The storage time of the resin is greatly influenced by the pure use of the phosphoric acid curing agent, and the resin can not be used after being dried for 2-4 weeks after the curing agent is added, or the resin has too high viscosity after being used for 5 times.
The existing resin impregnation process of the C/C composite material generally comprises the steps of directly pressurizing and impregnating after vacuumizing, and has no treatment on the surface of a material pore. Because the impregnated blank is of a porous structure, the specific surface area is large, and small molecules such as water molecules are easily adsorbed on the surfaces of the pores, so that the impregnation of the lipophilic resin is adversely affected. The pores are not subjected to interface pretreatment, so that the binding force between the resin and the carbon fiber/deposited carbon is poor, and the impregnation efficiency and the mechanical properties of the material are affected.
Disclosure of Invention
Aiming at the defects of the prior art, the application aims to provide a method for quickly compacting a carbon-carbon composite material.
In order to achieve the above purpose, the present application adopts the following technical scheme:
the application relates to a method for quickly compacting a carbon-carbon composite material, which comprises the steps of carrying out heat treatment on a carbon blank to obtain a carbon-carbon porous body, soaking the carbon-carbon porous body in phosphoric acid aqueous solution, obtaining the carbon-carbon porous body subjected to interface pretreatment after the soaking is finished, placing the carbon-carbon porous body subjected to interface pretreatment in an impregnating tank of an impregnating device, vacuumizing, then sucking an impregnating agent into the impregnating tank, and carrying out pressurized impregnation, curing, carbonization and graphitization; repeating the steps of pressurized impregnation, solidification, carbonization and graphitization until a compact carbon-carbon composite material is obtained; the impregnant comprises furfuryl ketone resin, phosphoric acid and zinc chloride, wherein the addition amount of the phosphoric acid is 1-10% of the weight of the furfuryl ketone resin, and the addition amount of the zinc chloride is 1-5% of the weight of the resin.
The application provides a method for quickly compacting a carbon-carbon composite material, which comprises the steps of firstly carrying out heat treatment on a carbon blank, carrying out clean treatment on volatile matters in chemical vapor deposition matrix carbon in the carbon blank, opening blocking holes in the process, soaking a carbon-carbon porous body in a phosphoric acid aqueous solution, and carrying out pretreatment on the interface of the carbon-carbon porous body by adopting phosphoric acid. The zinc chloride curing agent is a latent curing agent, the resin is not cured basically below 100 ℃, the viscosity of the resin is not increased, the resin can be cured at high temperature, the low viscosity of the resin can improve the depth of the resin penetrating into the material in the process of penetrating into the pores of the carbon/carbon composite material, the resin impregnation efficiency can be effectively improved, the curing speed of the resin at normal temperature can be slowed down, the resin use times and the storage time can be prolonged, and through the annular phase-locked process, the impregnation times of the carbon/carbon composite material can be reduced by 10% -40%, the mechanical property is integrally improved by 5% -20%, and the service life of the resin can be prolonged by 50% -100%.
However, the inventor finds that the formula of the impregnant needs to be effectively controlled, if the adding amount of phosphoric acid is too much, the effect of curing and crosslinking on improving the mechanical properties of the material is not obvious, the adding amount of phosphoric acid is linearly related to the viscosity of the resin, the viscosity is also increased, the impregnation effect is affected, the mechanical properties of the carbon-carbon composite material are reduced when the adding amount of phosphoric acid is too little, the viscosity of the resin is not affected any more when zinc chloride is added in a proper proportion, and the mechanical properties are continuously improved at the same time, however, compared with the phosphoric acid curing agent, the same zinc chloride content can cause the mechanical properties of the material to be slightly reduced, so that the adding amount of phosphoric acid and zinc chloride is controlled within the range of the application, so that the impregnation effect is optimal and the mechanical properties are optimal.
In the actual operation process, zinc chloride is dissolved in ethanol and then evenly mixed with furfuryl ketone resin and phosphoric acid to obtain the impregnant.
Preferably, the carbon-carbon blank is obtained by chemical vapor deposition of a carbon fiber preform, and the density of the carbon-carbon blank is 1.0-1.6 g/cm 3 。
In a preferred scheme, the temperature of the heat treatment is 2000-3000 ℃, preferably 2000-2300 ℃, and the time of the heat treatment is 1-3 h.
In a preferred scheme, in the phosphoric acid aqueous solution, the mass fraction of phosphoric acid is 5% -25%, and preferably 8% -20%.
The inventors have found that the mass fraction of phosphoric acid needs to be effectively controlled depending on the green density. If the mass fraction is too low, the introduced phosphoric acid content is too small, the activated crosslinking of the carbon blank is limited, and the improvement of the mechanical property of the material is influenced; if the mass fraction of phosphoric acid is too high, the impregnation efficiency is affected by the excessive amount of phosphoric acid finally cited.
Preferably, the soaking time is 0.5-2 h.
In the actual operation process, after the soaking is finished, vacuumizing and drying are carried out for 2-4 hours at 60-80 ℃ to obtain the carbon-carbon porous body subjected to interface pretreatment.
In a preferred scheme, the adding amount of phosphoric acid in the impregnant is 1-2.5% of the weight of the furfuryl ketone resin, and the adding amount of zinc chloride is 3-4% of the weight of the resin.
Preferably, the pressure of the pressurized impregnation is 1.0-8.0 MPa, preferably 3.9-4.2MPa, and the time is 2-6 h.
Preferably, the impregnating device comprises: the device comprises a vacuumizing system, a pressurizing system, resin tanks and impregnating tanks, wherein 3 impregnating tanks are respectively an a tank, a b tank and a c tank, 3 impregnating tanks are arranged in parallel with the resin tanks through a pipeline system, the pipeline system comprises a main pipeline and a plurality of branch pipelines, 3 impregnating tanks are connected in parallel with the main pipeline through corresponding branch pipelines, a differential pressure control valve is arranged on the main pipeline between two adjacent impregnating tanks, a vacuum valve is arranged on the main pipeline between the resin tanks and the impregnating tanks close to the resin tanks, and the vacuumizing system and the pressurizing system are respectively connected with each impregnating tank; the bottom of the dipping tank is provided with a liquid level test tank; when one of the impregnation tanks works in impregnation, one of the rest impregnation tanks is a buffer tank and one of the rest impregnation tanks is a standby tank, the pressure difference between the standby tank and the impregnation tank in impregnation is 0.1-0.3 MPa, and the pressure in the buffer tank is normal pressure;
dividing the carbon-carbon porous body subjected to interface pretreatment into three batches, respectively placing the three batches in a tank a, a tank b and a tank c, firstly adding an impregnant into a resin tank, and uniformly stirring; then vacuumizing the tank a, discharging the impregnant into the tank a from the resin tank, stopping vacuumizing when the liquid level of the resin submerges the product, filling high-pressure nitrogen into the tank a to enable the pressure in the tank a to reach 1.0-8.0 MPa, filling high-pressure nitrogen into the tank b to enable the pressure in the tank b to be smaller than the pressure in the tank a by 0.1-0.3 MPa, controlling the pressure in the tank c to be the same as the pressure in the resin tank at the moment, opening a differential pressure control valve between the tank a and the tank b after the tank a is subjected to pressurized impregnation for 2-6h to enable the redundant resin in the tank a to be pressed into the tank b, starting pressurizing, heating and solidifying the tank a, boosting the tank b to 1.0-8.0 MPa, starting the impregnation, and boosting the tank c to be 0.1-0.3 MPa smaller than the pressure in the tank b to serve as a standby tank; after the curing of the tank a is completed, the pressure is released to the normal pressure state, and the cured product is discharged; after the impregnation of the tank b is finished, the redundant resin is transferred to the tank c, and the operation is the same as that of transferring the tank a to the tank b; thereby realizing cyclic impregnation.
In the preferred scheme, the impregnating unit is through parallelly connected a plurality of impregnating tanks that set up, after the impregnating job in one of them impregnating tank accomplishes, need not to release pressure to normal pressure state, just can discharge the unnecessary resin in the jar to in the impregnating tank rather than adjacent, for the advantage that uses single impregnating tank among the prior art lies in: the pressure relief process between impregnation and solidification is reduced, the pressure relief reverse osmosis phenomenon in the impregnation solidification process is prevented, the performance of a product is guaranteed, continuous circulation production can be realized, the efficiency is improved, the cost is reduced, a plurality of impregnation tanks can play a role in buffering, and the safety coefficient of the whole impregnation device is improved.
Further preferably, the liquid level test tank comprises a connecting pipe, a pressure tank and a discharge pipe, one end of the connecting pipe is connected with the impregnating tank, the other end of the connecting pipe is connected with the pressure tank, the discharge pipe is arranged at the bottom of the pressure tank, a first manual switch valve is arranged on the connecting pipe, and a second manual switch valve is arranged on the discharge pipe.
Further preferably, the evacuation system comprises a vacuum pump, a valve and a vacuum line.
Further preferably, the pressurization system comprises a high pressure nitrogen tank, a valve and a pressurization pipeline.
In a preferred scheme, the curing temperature is 60-200 ℃ and the curing time is 6-15 h.
In a preferred scheme, the carbonization process is to raise the temperature to 850-950 ℃ at a heating rate of less than or equal to 1 ℃/min, and then to lower the temperature.
In a preferred scheme, the graphitization temperature is 2000-3000 ℃ and the graphitization time is 10-25 h.
In a preferred scheme, the times of repeated pressurized impregnation-solidification-carbonization-graphitization are 2-5 times.
Preferably, the density of the carbon-carbon composite material is 1.80-1.95 g/cm 3 。
Advantageous effects
The application provides a method for quickly compacting a carbon-carbon composite material, which comprises the steps of firstly carrying out heat treatment on a carbon blank, carrying out clean treatment on volatile matters in chemical vapor deposition matrix carbon in the blank, opening blocking holes in the process, soaking a carbon-carbon porous body in a phosphoric acid aqueous solution, and carrying out pretreatment on the interface of the carbon-carbon porous body by adopting phosphoric acid. The zinc chloride curing agent has the main function of reducing the viscosity of the resin after the resin is added with the curing agent, is a curing agent component capable of diluting the resin, has the potential of basically not curing the resin at normal temperature, cures the resin at high temperature, can improve the depth of the resin penetrating into the inside of the material in the process of penetrating the resin into the pores of the carbon/carbon composite material, can effectively improve the resin impregnation efficiency, can slow down the curing speed of the resin at normal temperature, and can prolong the use times and the storage time of the resin.
In addition, the impregnating device of the application is provided with the plurality of impregnating tanks in parallel, and when the impregnating operation in one of the impregnating tanks is completed, the impregnating device can discharge the redundant resin in the tank into the adjacent impregnating tank without pressure relief to normal pressure, and has the advantages that compared with the prior art that a single impregnating tank is used: the pressure relief process between impregnation and solidification is reduced, the pressure relief reverse osmosis phenomenon in the impregnation solidification process is prevented, the performance of a product is guaranteed, continuous circulation production can be realized, the efficiency is improved, the cost is reduced, a plurality of impregnation tanks can play a role in buffering, and the safety coefficient of the whole impregnation device is improved.
Through the annular buckling process, the impregnation times of the carbon-carbon composite material can be reduced by 10% -40%, the mechanical property is integrally improved by 5% -20%, the service life of the resin can be prolonged by 50% -100%, and meanwhile, through nondestructive detection, the microcrack and layering conditions of the finished product of the carbon/carbon composite material are reduced by more than 20%.
Drawings
Fig. 1 is a schematic structural view of an impregnating apparatus.
Wherein, each reference sign in the figure: 1. a resin tank; 2. an impregnation tank; respectively an a tank, a b tank, a c tank, 3 and a main pipeline; 4. a branch pipe; 5. a vacuum valve; 6. a differential pressure control valve; 7. a vacuum pumping system; 8. a pressurization system; 9. a liquid level test tank.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the application is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
It will be understood that when an element is referred to as being "mounted" or "disposed" on another element, it can be directly on the other element or be indirectly on the other element. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or be indirectly connected to the other element.
It is to be understood that the terms "length," "width," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are merely for convenience in describing and simplifying the description based on the orientation or positional relationship shown in the drawings, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus are not to be construed as limiting the application.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present application, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
As shown in fig. 1, an impregnating apparatus comprising a plurality of impregnating tanks according to the present application will now be described. The impregnation device comprises: the vacuum pumping system 7, the pressurizing system 8, the resin tank 1 and the impregnating tank 2 are all of the structures of the vacuum pumping system 7, the pressurizing system 8, the resin tank 1 and the impregnating tank 2 by adopting the existing equipment.
Specifically, three impregnating tanks 2 are respectively an a tank, a b tank and a c tank, the three impregnating tanks 2 are arranged in parallel with the resin tank 1 through a pipeline system, the pipeline system comprises a main pipeline 3 and a plurality of branch pipelines 4, the number of the branch pipelines 4 is the same as that of the impregnating tanks 2, the plurality of impregnating tanks 2 are connected in parallel with the main pipeline 3 through corresponding branch pipelines 4, and the resin tank 1 is connected with one end of the main pipeline 3. Wherein, a differential pressure control valve 6 is arranged on a main pipeline 3 between two adjacent impregnating tanks 2, a vacuum valve 5 is arranged on the main pipeline 3 between the resin tank 1 and the impregnating tank 2 close to the resin tank, and a vacuumizing system 7 and a pressurizing system 8 are respectively connected with each impregnating tank 2. The vacuum valve 5, the differential pressure control valve 6, the pressurizing system 8 and the vacuumizing system 7 are matched with each other, so that the pressure in each impregnating tank 2 is in different states, for example, the pressures of two adjacent impregnating tanks 2 are relatively close, for example, the pressure difference is 0.2MPa, and therefore, after one of the impregnating tanks 2 finishes impregnating operation, the residual resin in the impregnating tank 2 can be discharged into the adjacent impregnating tank 2 without pressure relief.
In this embodiment, through setting up 3 impregnation jars 2 in parallel, after the impregnation work in one of them impregnation jar 2 is accomplished, need not to release to normal pressure state, just can discharge the unnecessary resin in the jar into the impregnation jar 2 adjacent to it in, for the single impregnation jar that uses in the prior art: the pressure relief process between impregnation and solidification is reduced, the pressure relief reverse osmosis phenomenon in the impregnation solidification process is prevented, the performance of the product is guaranteed, continuous circulation production can be realized, the efficiency is improved, the cost is reduced, and the plurality of impregnation tanks 2 can play a role in buffering, so that the safety coefficient of the whole impregnation device is improved.
In this embodiment, the bottom of each impregnation tank 2 is provided with a liquid level test tank 9, and the liquid level test tank 9 is used for determining whether the resin remaining in the impregnation tank 2 is completely discharged. Specifically, liquid level test tank 9 includes connecting pipe, overhead tank and row material pipe, and the one end and the flooding jar 2 of connecting pipe are connected, and the other end is connected with the overhead tank, and row material pipe sets up in the bottom of overhead tank, is equipped with first manual ooff valve on the connecting pipe, is equipped with the manual ooff valve of second on the row material pipe. When it is required to detect whether the resin in the impregnation tank 2 is exhausted, the first manual switch is turned on firstly, so that the resin in the impregnation tank 2 flows into the pressure tank under the self gravity, after waiting for a certain time, the first manual switch is turned off, and then the second manual switch is turned on, so that the resin in the pressure tank is exhausted through the exhaust pipe, and whether the resin in the impregnation tank 2 is exhausted is determined according to the resin exhausted through the exhaust pipe. The liquid level test tank 9 is operated for a plurality of times according to a certain time interval to ensure that no resin remains in the impregnation tank 2 and avoid the phenomenon that a pipeline is blocked by the resin in the subsequent temperature rise curing process.
In this embodiment, when one of the impregnation tanks 2 is in impregnation operation, at least one of the remaining impregnation tanks 2 is a buffer tank and one of the impregnation tanks 2 is a standby tank, wherein the pressure difference between the standby tank and the impregnation tank 2 in impregnation operation is 0.1-0.3 MPa, and the pressure in the buffer tank is normal pressure.
In the application, the evacuation system 7 comprises a vacuum pump, valves and vacuum lines. The pressurization system 8 includes a high pressure nitrogen tank, valves, and pressurization piping. The vacuumizing system 7 and the pressurizing system 8 can be arranged in one set, or can be arranged in a plurality of sets; when the vacuum pipeline is provided with one set, a plurality of valves are arranged on the vacuum pipeline and the valves on the pressurizing pipeline are arranged corresponding to the impregnating tanks 2, so that the pressurizing system 8 and the vacuumizing system 7 can independently vacuumize and pressurize the corresponding impregnating tanks 2.
The resin tank 1 and the three impregnating tanks 2 are arranged in parallel, the first impregnating tank 2 close to the resin tank 1 is a tank, the middle impregnating tank 2 is b tank, and the impregnating tank 2 far away from the resin tank 1 is c tank.
The specific dipping process by the dipping device is as follows:
firstly, adding resin and a curing agent into a resin tank 1, and uniformly stirring;
secondly, filling products in the tank a, immersing and vacuumizing the tank a by a vacuumizing system 7, opening a vacuum valve 5, discharging resin into the tank a from the resin tank 1, immersing the products in the liquid level of the resin, and closing the vacuum valve 5;
thirdly, filling high-pressure nitrogen into the tank a by a pressurizing system 8 to enable the pressure in the tank a to reach 1.0-8.0 MPa, and starting pressurizing and soaking for 2-6 hours;
fourthly, filling products into the tank b, and filling high-pressure nitrogen into the tank b by the pressurizing system 8 to ensure that the pressure in the tank b is 0.1-0.3 MPa smaller than that in the tank a, wherein the pressure in the tank c and the pressure in the resin tank 1 are the same and are 0MPa as standby tanks, the tank c is used as a buffer tank, and when pressure control fails, the pressure can be directly released to the tank c to avoid the jump of a safety valve or a pressure release path is added when the safety valve fails, so that the safety is ensured;
fifthly, after the product in the tank a is immersed, opening a pressure difference control valve 6 between the tank a and the tank b, and pressing redundant resin in the tank a into the tank b by utilizing the pressure difference between the tank a and the tank b;
step six, tank a determines whether the redundant resin is exhausted through a liquid level test tank 9, and after the resin is exhausted, the differential pressure control valve 6 is closed;
seventh, the tank a starts to be pressurized, heated and solidified, the tank b starts to be soaked after being pressurized to 1.0-8.0 MPa, and the tank c is pressurized to 0.1-0.3 MPa lower than the tank b and is used as a standby tank;
eighth, after the solidification of the tank a is completed, the pressure is relieved to a normal pressure state, and the product is discharged;
step nine, after the impregnation of the tank b is finished, the redundant resin is transferred to the tank c, and the operation is the same as the operation of transferring the tank a to the tank b; similarly, the operation of tank c is the same, thus achieving a cyclic impregnation of the product.
Each differential pressure control valve 6 is an electric control valve, so that when the pressure difference is smaller than 0.2MPa, the differential pressure control valve 6 is opened, and when the pressure difference is larger than 0.2MPa, the differential pressure control valve 6 is closed; the purpose of this is to prevent the pressure difference from being too great, so that the resin flow rate is too high to break up the product.
Because a plurality of impregnating tanks 2 are arranged in parallel, the recycling of resin is realized, raw materials are saved, the continuous production can greatly speed up the production rhythm, and a single batch of resin can impregnate more products. Meanwhile, the pressure relief is reduced for 1 time, and the high-pressure nitrogen consumption is saved.
Example 1
This example employs an impregnating apparatus comprising a single resin tank and impregnating tank.
Zinc chloride is dissolved in ethanol and then evenly mixed with furfuryl ketone resin and phosphoric acid in a resin tank to obtain an impregnant, wherein the impregnant comprises the furfuryl ketone resin, phosphoric acid and zinc chloride, the adding amount of the phosphoric acid is 2% of the weight of the furfuryl ketone resin, and the adding amount of the zinc chloride is 3% of the weight of the resin.
The density was set at 0.45g/cm 3 The carbon fiber preform of (2) is subjected to chemical vapor deposition to obtain a carbon fiber preform with a density of 1.33g/cm 3 Performing heat treatment on the carbon-carbon blank for 1h at 2000 ℃ to obtain a carbon-carbon porous body, soaking the carbon-carbon porous body in phosphoric acid aqueous solution with the mass of 10% of phosphoric acid, obtaining an interface-pretreated carbon-carbon porous body after soaking, placing the interface-pretreated carbon-carbon porous body in an impregnating tank of an impregnating device, heating, vacuumizing and drying, sucking an impregnating agent into the impregnating tank, pressurizing and impregnating for 4h at 4.0MPa, directly heating to 200 ℃ in the impregnating tank for curing for 10h, slowly heating to 900 ℃ at a heating rate of less than or equal to 1 ℃ under nitrogen atmosphere, carbonizing, immediately cooling, and graphitizing at 2000 ℃ under argon atmosphere; repeated pressurizing dipping-solidifying-carbonizing-graphitizing for 5 times to obtain compact density of 1.88g/cm 3 A carbon-carbon composite material.
The impregnant used in this example showed only a slight increase in viscosity after repeating 5 times, and the impregnant which was not completely used up could be used for impregnating other batches of carbon-carbon porous bodies.
The carbon-carbon composite material obtained in the detection example 1 has the radial compression strength of 111MPa, the axial compression strength of 247MPa, the radial tensile strength of 148MPa, the axial tensile strength of 85MPa, the radial shearing strength of 67MPa and the axial shearing strength of 42MPa.
Example 2
The impregnating device provided by the application is used for impregnating by arranging a plurality of impregnating tanks in parallel.
Zinc chloride is firstly dissolved in ethanol, and then is uniformly mixed with furfuryl ketone resin and phosphoric acid in a resin tank to obtain an impregnant, wherein the impregnant comprises the furfuryl ketone resin, phosphoric acid and zinc chloride, the adding amount of the phosphoric acid is 2.5% of the weight of the furfuryl ketone resin, and the adding amount of the zinc chloride is 3% of the weight of the resin.
The density was set at 0.45g/cm 3 The carbon fiber preform of (2) is subjected to chemical vapor deposition to obtain a carbon fiber preform with a density of 1.25g/cm 3 Performing heat treatment on the carbon-carbon blank for 1h at 2000 ℃ to obtain a carbon-carbon porous body, soaking the carbon-carbon porous body in a phosphoric acid aqueous solution with the mass of 8% of phosphoric acid, obtaining the carbon-carbon porous body subjected to interface pretreatment after the soaking is finished, dividing the carbon-carbon porous body subjected to interface pretreatment into three batches, respectively placing the three batches of carbon-carbon porous bodies in a tank, a tank b tank and a tank c, adding an impregnant into a resin tank, and uniformly stirring; then vacuuming the tank a, discharging the impregnant into the tank a from the resin tank, stopping vacuuming when the liquid level of the resin submerges the product, filling high-pressure nitrogen into the tank a to enable the pressure in the tank a to reach 4.0MPa, simultaneously filling high-pressure nitrogen into the tank b to enable the pressure in the tank b to be smaller than the pressure in the tank a by 0.2MPa, controlling the pressure in the tank c to be the same as the pressure of the resin tank at the moment, opening a differential pressure control valve between the tank a and the tank b after the tank a is in pressurized impregnation for 4h, enabling the redundant resin in the tank a to be pressed into the tank b, starting the pressurized heating and curing of the tank a (10 h is cured at 200 ℃, starting the impregnation after the tank b is in pressurized heating up to 4.0MPa, taking the tank b as a standby tank after the tank c is in pressurized up to be 0.1-0.3 MPa smaller than the pressure in the tank b, discharging the cured product after the tank a is in the normal pressure state, transferring the redundant resin into the tank c after the tank b is in the impregnation is completed, and operating the same as the tank a is transferred into the tank bThe method comprises the steps of carrying out a first treatment on the surface of the So as to realize cyclic impregnation and solidification, all three batches of obtained solidified products are carbonized at 900 ℃ at the heating rate of less than or equal to 1 ℃ in nitrogen atmosphere, then cooled, and finally graphitized at 2000 ℃ in argon atmosphere; repeated pressurizing dipping-solidifying-carbonizing-graphitizing for 4 times to obtain compact density of 1.87g/cm 3 A carbon-carbon composite material.
The impregnant used in this example showed little change in viscosity after repeating 4 times, and the impregnant which was not completely used up could be used for impregnating other batches of carbon-carbon porous bodies.
Carbon-carbon composite material obtained in detection example 2: the radial compression strength is 117MPa, the axial compression strength is 258MPa, the radial tensile strength is 152MPa, the axial tensile strength is 90MPa, the radial shearing strength is 72MPa, and the axial shearing strength is 45MPa.
Example 3
The impregnating device provided by the application is used for impregnating by arranging a plurality of impregnating tanks in parallel.
Zinc chloride is firstly dissolved in ethanol, and then is uniformly mixed with furfuryl ketone resin and phosphoric acid in a resin tank to obtain an impregnant, wherein the impregnant comprises the furfuryl ketone resin, phosphoric acid and zinc chloride, the adding amount of the phosphoric acid is 1% of the weight of the furfuryl ketone resin, and the adding amount of the zinc chloride is 4% of the weight of the resin.
The density was set at 0.40g/cm 3 The carbon fiber preform of (2) is subjected to chemical vapor deposition to obtain a carbon fiber preform with a density of 1.58g/cm 3 Performing heat treatment on the carbon-carbon blank for 1h at 2000 ℃ to obtain a carbon-carbon porous body, soaking the carbon-carbon porous body in a phosphoric acid aqueous solution with the mass of 20% of phosphoric acid, obtaining the carbon-carbon porous body subjected to interface pretreatment after the soaking is finished, dividing the carbon-carbon porous body subjected to interface pretreatment into three batches, respectively placing the three batches of carbon-carbon porous bodies in a tank, a tank b tank and a tank c, adding an impregnant into a resin tank, and uniformly stirring; then vacuuming the tank a to discharge the impregnant into the tank a from the resin tank, stopping vacuuming when the liquid level of the resin submerges the product, filling high-pressure nitrogen into the tank a to ensure that the pressure in the tank a reaches 4.0MPa, and simultaneously filling high-pressure nitrogen into the tank b to ensure that the pressure in the tank b is smaller than the pressure in the tank a by 0.2MPa, and controlling the pressure in the tank c and the pressure in the resin tank at the momentThe pressure is the same, after the tank a is pressurized and immersed for 6 hours, a differential pressure control valve between the tank a and the tank b is opened, so that redundant resin in the tank a is pressed into the tank b, the tank a begins to be pressurized, heated and solidified (200 ℃ and solidified for 10 hours), the tank b is pressurized to 4.0MPa and immersed, and the tank c is pressurized to be 0.2MPa smaller than the pressure of the tank b and serves as a standby tank; after the curing of the tank a is completed, the pressure is released to the normal pressure state, and the cured product is discharged; after the impregnation of the tank b is finished, the redundant resin is transferred to the tank c, and the operation is the same as that of transferring the tank a to the tank b; so as to realize cyclic impregnation and solidification, and all three batches of obtained solidified products are placed in a nitrogen atmosphere to be carbonized at 900 ℃ for 45 hours, and finally graphitized at 2000 ℃ in an argon atmosphere; repeated pressurizing dipping-solidifying-carbonizing-graphitizing for 2 times to obtain compact density of 1.84g/cm 3 A carbon-carbon composite material.
Carbon-carbon composite material obtained in detection example 3: the radial compression strength is 132MPa, the axial compression strength is 282MPa, the radial tensile strength is 175MPa, the axial tensile strength is 106MPa, the radial shearing strength is 87MPa, and the axial shearing strength is 61MPa.
Comparative example 1
Otherwise, the same conditions as in example 1 were employed, except that no zinc chloride was added to the impregnating agent, and the impregnation under repeated pressure, curing, carbonization and graphitization were conducted to obtain a dense density of 1.88g/cm 3 A carbon-carbon composite material.
The mechanical properties of the carbon-carbon composite material obtained in the final comparative example 1 are as follows: compression strength 104MPa, axial compression strength 223MPa, radial tensile strength 131MPa, axial tensile strength 82MPa, radial shear strength 61MPa and axial shear strength 39MPa.
Comparative example 2
Other conditions were the same as in example 1 except that no phosphoric acid pretreatment was used, and the density obtained in final comparative example 2 was 1.88g/cm 3 The mechanical properties of the carbon-carbon composite material are as follows: the radial compression strength is 97MPa, the axial compression strength is 205MPa, the radial tensile strength is 127MPa, the axial tensile strength is 78MPa, the radial shearing strength is 58MPa, and the axial shearing strength is 36MPa.
Claims (8)
1. A method for quickly compacting a carbon-carbon composite material is characterized by comprising the following steps: carrying out heat treatment on the carbon-carbon blank to obtain a carbon-carbon porous body, soaking the carbon-carbon porous body in a phosphoric acid aqueous solution, obtaining an interface-pretreated carbon-carbon porous body after the soaking is finished, placing the interface-pretreated carbon-carbon porous body in an impregnating tank of an impregnating device, vacuumizing, sucking an impregnating agent into the impregnating tank, and carrying out pressurized impregnation, curing, carbonization and graphitization; repeating the steps of pressurized impregnation, solidification, carbonization and graphitization until a compact carbon-carbon composite material is obtained;
the carbon-carbon green body is obtained by chemical vapor deposition of a carbon fiber preform, and the density of the carbon-carbon green body is 1.0-1.6 g/cm 3 ；
In the phosphoric acid aqueous solution, the mass fraction of phosphoric acid is 5% -25%, and the soaking time is 0.5-2 h;
the impregnant comprises furfuryl ketone resin, phosphoric acid and zinc chloride, wherein the addition amount of the phosphoric acid is 1-10% of the weight of the furfuryl ketone resin, and the addition amount of the zinc chloride is 1-5% of the weight of the resin.
2. The method for rapid densification of a carbon-carbon composite material according to claim 1, wherein: the temperature of the heat treatment is 2000-3000 ℃, and the time of the heat treatment is 1-3 hours.
3. The method for rapid densification of a carbon-carbon composite material according to claim 1, wherein: the pressure of the pressurized impregnation is 1.0-8.0 MPa, and the time of the pressurized impregnation is 2-6 h.
4. The method for rapid densification of a carbon-carbon composite material according to claim 1, wherein: the impregnation device comprises: the device comprises a vacuumizing system, a pressurizing system, resin tanks and impregnating tanks, wherein 3 impregnating tanks are respectively an a tank, a b tank and a c tank, 3 impregnating tanks are arranged in parallel with the resin tanks through a pipeline system, the pipeline system comprises a main pipeline and a plurality of branch pipelines, 3 impregnating tanks are connected in parallel with the main pipeline through corresponding branch pipelines, a differential pressure control valve is arranged on the main pipeline between two adjacent impregnating tanks, a vacuum valve is arranged on the main pipeline between the resin tanks and the impregnating tanks close to the resin tanks, and the vacuumizing system and the pressurizing system are respectively connected with each impregnating tank; the bottom of the dipping tank is provided with a liquid level test tank; when one of the impregnation tanks works in impregnation, one of the rest impregnation tanks is a buffer tank and one of the rest impregnation tanks is a standby tank, the pressure difference between the standby tank and the impregnation tank in impregnation is 0.1-0.3 MPa, and the pressure in the buffer tank is normal pressure;
dividing the carbon-carbon porous body subjected to interface pretreatment into three batches, respectively placing the three batches in a tank a, a tank b and a tank c, firstly adding an impregnant into a resin tank, and uniformly stirring; then vacuumizing the tank a, discharging the impregnant into the tank a from the resin tank, stopping vacuumizing when the liquid level of the resin submerges the product, filling high-pressure nitrogen into the tank a to enable the pressure in the tank a to reach 1.0-8.0 MPa, filling high-pressure nitrogen into the tank b to enable the pressure in the tank b to be smaller than the pressure in the tank a by 0.1-0.3 MPa, controlling the pressure in the tank c to be the same as the pressure in the resin tank at the moment, opening a differential pressure control valve between the tank a and the tank b after the tank a is subjected to pressurized impregnation for 2-6h to enable the redundant resin in the tank a to be pressed into the tank b, starting pressurizing, heating and solidifying the tank a, boosting the tank b to 1.0-8.0 MPa, starting the impregnation, and boosting the tank c to be 0.1-0.3 MPa smaller than the pressure in the tank b to serve as a standby tank; after the curing of the tank a is completed, the pressure is released to the normal pressure state, and the cured product is discharged; after the impregnation of the tank b is finished, the redundant resin is transferred to the tank c, and the operation is the same as that of transferring the tank a to the tank b; thereby realizing cyclic impregnation.
5. The method for rapid densification of a carbon-carbon composite material according to claim 4, wherein:
the liquid level testing tank comprises a connecting pipe, a pressure tank and a discharge pipe, one end of the connecting pipe is connected with the dipping tank, the other end of the connecting pipe is connected with the pressure tank, the discharge pipe is arranged at the bottom of the pressure tank, a first manual switch valve is arranged on the connecting pipe, and a second manual switch valve is arranged on the discharge pipe;
the vacuumizing system comprises a vacuum pump, a valve and a vacuum pipeline;
the pressurizing system comprises a high-pressure nitrogen tank, a valve and a pressurizing pipeline.
6. The method for rapid densification of a carbon-carbon composite material according to claim 4, wherein: the curing temperature is 60-200 ℃, and the curing time is 6-15 h; the carbonization process is that the temperature rising rate is less than or equal to 1 ℃/min, the temperature rises to 850-950 ℃, the temperature is immediately reduced, the graphitization temperature is 2000-3000 ℃, and the graphitization time is 10-25 h.
7. The method for rapid densification of a carbon-carbon composite material according to claim 1, wherein: the times of repeated pressurizing dipping-solidifying-carbonizing-graphitizing are 2-5 times.
8. A method for rapid densification of a carbon-carbon composite material according to any one of claims 1-7, wherein: the density of the carbon-carbon composite material is 1.80-1.95 g/cm 3 。
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