CN114702330A - Densification method of carbon fiber preform - Google Patents
Densification method of carbon fiber preform Download PDFInfo
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- CN114702330A CN114702330A CN202210638377.4A CN202210638377A CN114702330A CN 114702330 A CN114702330 A CN 114702330A CN 202210638377 A CN202210638377 A CN 202210638377A CN 114702330 A CN114702330 A CN 114702330A
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- carbon fiber
- fiber preform
- carbon
- treatment
- powder
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 147
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 147
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 143
- 238000000034 method Methods 0.000 title claims abstract description 63
- 238000000280 densification Methods 0.000 title abstract description 36
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 72
- 239000011347 resin Substances 0.000 claims abstract description 64
- 229920005989 resin Polymers 0.000 claims abstract description 64
- 239000002131 composite material Substances 0.000 claims abstract description 61
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims abstract description 54
- 230000001070 adhesive effect Effects 0.000 claims abstract description 41
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- 230000008569 process Effects 0.000 claims abstract description 28
- 229960003638 dopamine Drugs 0.000 claims abstract description 27
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- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical compound OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 0.000 claims abstract description 17
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- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 claims abstract description 5
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- 238000001816 cooling Methods 0.000 claims description 18
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- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 11
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- 229910052882 wollastonite Inorganic materials 0.000 claims description 11
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 8
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- 230000000694 effects Effects 0.000 abstract description 33
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- RWOCXFPQPISTSD-UHFFFAOYSA-N 5-chloro-2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine Chemical compound O1C(C)(C)C(C)(C)OB1C1=CC=C(Cl)C=N1 RWOCXFPQPISTSD-UHFFFAOYSA-N 0.000 description 10
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 10
- 239000006087 Silane Coupling Agent Substances 0.000 description 8
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
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- 239000000835 fiber Substances 0.000 description 4
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
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Abstract
The invention discloses a densification method of a carbon fiber preform, which relates to the technical field of carbon fiber material forming processes and comprises the following steps: firstly, soaking, hot-pressing curing and carbonizing a carbon fiber preform to obtain a carbon-carbon plate, and then carrying out liquid-phase impregnation and carbonization; the soaking solution used in the soaking treatment process comprises resin adhesive compound solution; the raw materials of the resin adhesive composite liquid comprise a resin adhesive, a diluent, a filler and carbon powder; the impregnant used in the liquid phase impregnation treatment process consists of resin gum and a diluent; the carbon fiber preform is subjected to dipping treatment by using a dopamine solution containing iminodiacetic acid before the dipping treatment. The densification method provided by the invention has more excellent densification effect, the treatment period is obviously reduced, the density of the treated carbon fiber composite material is effectively improved, the interlayer bonding condition is improved, and the mechanical property is obviously enhanced; meanwhile, the heat-conducting property of the carbon fiber composite material is obviously improved.
Description
Technical Field
The invention belongs to the technical field of carbon fiber material forming processes, and particularly relates to a densification method of a carbon fiber preform.
Background
The carbon/carbon plate has the characteristics of strong acid and strong alkali resistance, high mechanical property, long replacement period and the like, can completely replace graphite and ceramic material parts, is used as a corrosion-resistant key part in high-temperature-resistant equipment, and is widely applied to the field of chemical high-temperature equipment. The high-temperature-resistant, high-strength and high-density carbon fiber plate is generally formed by repeatedly depositing a basic carbon fiber material in a needling and CVD furnace for many times or carbonizing a carbon fiber fabric in a carbonization furnace after bonding and vacuum gum dipping layer by layer.
The liquid phase impregnation process is a common densification process technology for C/C composite materials, and is a process of impregnating and permeating liquid hydrocarbon precursors into a prefabricated body under a certain temperature and pressure environment, filling pores, and cracking under a vacuum high-temperature condition to generate matrix carbon. The existing liquid-phase impregnation carbonization densification process takes pitch or resin as an impregnant, adopts a liquid-phase impregnation method to prepare a C/C composite material, and comprises an impregnation step and a high-temperature carbonization step, wherein in the impregnation step, the impregnation pitch or resin-embedded carbon fiber preform is loaded into a pressurized impregnation device and impregnated at a certain temperature and pressure; in the high-temperature carbonization step, the impregnated carbon fiber preform is taken out from the impregnant for carbonization, so that the densification treatment of the C/C material in one period is completed, and a plurality of periods are repeated until the carbon fiber preform reaches the required density. In the high-temperature carbonization step, the pitch or resin impregnated into the carbon fiber preform may be partially discharged from the preform due to the release of the impregnation pressure and the gas pressure generated during pyrolysis, which may result in a decrease in the impregnation efficiency of the material and an increase in the treatment period.
Disclosure of Invention
The invention aims to provide a densification method of a carbon fiber preform, which has more excellent densification effect, obviously reduces the treatment period, effectively improves the density of the treated carbon fiber composite material, improves the interlayer bonding condition and obviously enhances the mechanical property; meanwhile, the heat-conducting property of the carbon fiber composite material is obviously improved.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a method of densifying a carbon fiber preform, comprising: firstly, carrying out soaking treatment, hot-pressing curing and carbonization treatment on a carbon fiber preform to obtain a carbon-carbon plate, and then carrying out liquid-phase impregnation treatment and carbonization treatment; the soaking solution used in the soaking treatment process comprises resin adhesive compound solution; the raw materials of the resin adhesive composite liquid comprise a resin adhesive, a diluent, a filler and carbon powder; the filler comprises at least one of wollastonite powder and black talcum powder, diatomite and barium sulfate; the impregnant used in the liquid phase impregnation treatment process comprises resin glue solution which consists of resin glue and thinner. According to the invention, a liquid-phase impregnation process is adopted to carry out densification treatment on the carbon fiber preform, and the filler is added into the resin glue solution after soaking treatment, so that the carbon fiber preform has high specific surface area and high activation, is uniformly dispersed in a resin matrix and can effectively adsorb matrix molecular chains to form physical cross-linking points, and the bonding force in the resin glue is effectively enhanced; and at the interface of the carbon fiber and the resin adhesive, the physical cross-linking points can play a certain role of 'anchoring', so that the interface bonding property is improved, and further, the mechanical property of the carbon fiber composite material can be effectively improved. Similarly, the addition of the nano-scale carbon powder can improve the carbon residue rate of the composite material after high-temperature sintering and improve the overall density while generating the same effect.
Specifically, the resin adhesive includes one of phenolic resin, epoxy resin, and furan resin.
Specifically, the diluent comprises 60-80% ethanol.
Specifically, the carbon powder is in a nanometer level.
Specifically, the resin glue solution comprises, by weight, 4-10 parts of resin glue, 20-60 parts of diluent, 6-15 parts of filler and 1-5 parts of carbon powder.
Specifically, the density of the carbon fiber preform is 0.4-0.8 g/cm3。
Preferably, the carbon fiber preform is pretreated, that is, the carbon fiber preform is subjected to an impregnation treatment with a dopamine solution containing iminodiacetic acid before the liquid-phase impregnation treatment.
Specifically, the pretreatment operation of the carbon fiber preform includes:
dissolving dopamine in a Tris solution (pH 8-9) with the concentration of 8-10 mM to obtain a dopamine solution with the concentration of 2-3 mg/mL, adding iminodiacetic acid (the addition amount is 4-6 mg/mL), then soaking the dopamine solution in a carbon fiber preform for 24-32 h, taking out the dopamine solution, and draining to obtain a pretreated carbon fiber preform. According to the invention, the pretreatment method of dipping the carbon fiber preform by the dopamine solution is adopted, and the dopamine active layer is wrapped on the surface of the carbon fiber by utilizing the structural characteristics of dopamine, so that the problem of the interface between the carbon fiber and the resin adhesive can be effectively improved, the resin adhesive can be remained among carbon fiber pores as much as possible through partial physical/chemical actions in the dipping process, and the dipping effect is improved. Meanwhile, iminodiacetic acid is added into a dopamine solution, so that the functional activity of the surface of the carbon fiber can be further increased, the iminodiacetic acid can be attached to the surface of the carbon fiber through the wrapping effect of a polydopamine layer or the effects of hydrogen bonds, chemical bonds and the like, a certain 'bridge' effect is achieved, and during soaking, active functional groups on the surface of the carbon fiber can be subjected to physical or chemical action force, so that resin glue can be better immersed into gaps of the carbon fiber preform layer, the residual quantity of the resin glue is obviously increased, the soaking efficiency is greatly improved, the densification period is shortened, the rapid densification of the C/C material is realized, and the density of the carbon fiber composite material is obviously improved; and the interface effect of the carbon fiber and the resin adhesive is effectively improved, the interlaminar shear strength is obviously enhanced, and the interface bonding condition is obviously improved. Meanwhile, the mechanical property of the carbon fiber composite material is obviously improved, and the compressive strength of the carbon fiber composite material is obviously enhanced.
Furthermore, the resin glue solution raw material also comprises 0.5-2 parts by weight of p-toluenesulfonic acid.
Specifically, the soaking treatment process comprises the following steps: soaking the carbon fiber preform in the raw material of the resin adhesive composite liquid for not less than 5 hours;
the hot-pressing curing process comprises the following steps: under the pressure condition of 5-15 MPa, heating the temperature from 65-80 ℃ to 150-180 ℃ at the heating rate of 3-5 ℃/min, preserving the temperature for 5-10 h, and naturally cooling to 60-80 ℃.
Specifically, the conditions of the liquid-phase impregnation treatment include: under the vacuum condition, setting the pressure to be 1-5 MPa, the temperature to be 30-50 ℃, and the dipping time to be 1.5-3 h; then heating to 180-220 ℃ at a heating rate of 35-45 ℃/h, and curing for 2-4 h; and then naturally cooling to room temperature.
Specifically, the carbonization treatment process comprises the following steps: under the protection of inert gas, heating the temperature from 20-30 ℃ to 750-850 ℃ at a heating rate of 24-26 ℃/h, and keeping the temperature for 3-5 h at constant temperature; then raising the temperature to 1000-1100 ℃ at a heating rate of 40-45 ℃/h, and keeping the temperature for 2-4 h; then, cooling to 600-700 ℃ at a cooling rate of 40-50 ℃/h; and then cooling to 300-350 ℃ at a cooling rate of 30-40 ℃/h, and then naturally cooling to below 100 ℃.
Specifically, the mass ratio of the resin glue to the diluent in the resin glue solution is 1:3 to 5.
Specifically, the mass ratio of the wollastonite powder to the black talcum powder to the diatomite to the barium sulfate is 0.6-1: 0.4-0.8: 1: 0.5-0.7.
Specifically, the impregnation step and the carbonization step are complete treatment cycles, the next treatment cycle is started after the carbonization step is carried out, the impregnation step is carried out again, and the treatment is repeated until the density of the carbon fiber plate reaches the expected density.
The carbon fiber preform includes: the net-shaped tire comprises net-shaped tire layers and carbon fiber layers, wherein the carbon fiber layers are arranged between every two adjacent net-shaped tire layers at intervals and are compounded through the needling effect; wherein, the net-shaped layer is made of chopped carbon fiber through scattering, carding, net-laying and needling; the carbon fiber filament layer is obtained by spreading and ageing carbon fiber tows.
Specifically, the carbon fiber tow pavement comprises single-layer carbon fiber tow one-way pavement and/or double-layer carbon fiber tow two-way interweaving pavement.
More preferably, the self-dispersing carbon powder is used instead of the carbon powder in the raw material of the resin adhesive composite liquid.
Specifically, the preparation method of the self-dispersing carbon powder comprises the following steps: the self-dispersing carbon powder is obtained by chemically modifying the surface of carbon powder by adopting a silane coupling agent and 5-chloropyridine-2-boric acid pinacol ester. According to the invention, the silane coupling agent and 5-chloropyridine-2-boronic acid pinacol ester are adopted to functionally modify the surface of the carbon powder to obtain the high-activity nano carbon powder, which can be well and uniformly dispersed in a resin matrix, so that the problems of carbon powder precipitation phenomenon, easy agglomeration of the nano carbon powder and the like in the soaking process are solved; the bonding force in the resin adhesive is improved by generating beneficial influence on the network structure of the resin adhesive, a more stable and compact network structure is formed, the densification effect is enhanced, and the density of the carbon fiber composite material is obviously increased; meanwhile, the mechanical property of the carbon fiber composite material is effectively improved. And more physical cross-linking points can be formed on the interface of the resin adhesive and the carbon fibers by the self-dispersing carbon powder, so that the interface bonding strength of the resin adhesive and the carbon fibers is increased, the interlaminar shear strength is obviously enhanced, and the interface bonding condition is effectively improved. In addition, the organic compound containing the boron element is introduced from the surface of the dispersed carbon powder and enters the carbon structure, so that the crystallization of the carbon material in the graphitization process can be promoted, the whole graphite structure of the material is improved, the heat conductivity of the carbon fiber composite material is further effectively improved, and the heat conductivity coefficient is obviously increased.
Further, the preparation method of the self-dispersing carbon powder specifically comprises the following steps:
dissolving KH550 and ammonia water in an ethanol solution with the concentration of 85-95%, adding carbon powder, performing ultrasonic treatment for 20-40 min, then stirring for 20-24 h at the temperature of 40-45 ℃, centrifuging, washing with ethanol for 3-5 times, drying for 8-12 h at the temperature of 50-60 ℃, and grinding to obtain surface-treated carbon powder;
dissolving 5-chloropyridine-2-boronic acid pinacol ester in acetone at the concentration of 0.03-0.05 g/mL, adding surface-treated carbon powder, adjusting the pH to 5.5-6.5 by using sodium carbonate with the concentration of 1.2-1.5M, stirring for 2-4 hours at the temperature of 40 ℃, centrifuging, washing a mixed solution of methanol and ethanol (v/v, 1: 1-1.5) for 3-5 times, and drying at the temperature of 55-60 ℃ to obtain the self-dispersing carbon powder.
Specifically, the mass ratio of the KH550 to the ammonia water is 1: 0.1-0.2; the mass ratio of the KH550 to the ethanol solution is 1: 36-42; the mass ratio of the carbon powder to the KH550 is 1: 0.5-0.6.
Specifically, the mass ratio of the carbon powder subjected to surface treatment to the 5-chloropyridine-2-boronic acid pinacol ester is 1: 1-1.3.
Compared with the prior art, the invention has the following beneficial effects:
according to the densification method provided by the invention, the carbon fiber preform is soaked in the dopamine solution containing iminodiacetic acid in advance, so that resin glue enters and remains in gaps of the carbon fiber preform as much as possible during soaking, the soaking efficiency is greatly improved, and the density of the carbon fiber composite material is obviously improved; the bonding condition of the carbon fiber and resin adhesive interface is effectively improved, and the interlaminar shear strength is obviously enhanced; and the mechanical property of the carbon fiber composite material is obviously improved, and the compressive strength of the carbon fiber composite material is obviously enhanced. Meanwhile, the surface of the carbon powder is functionally modified by adopting a silane coupling agent and 5-chloropyridine-2-boronic acid pinacol ester, so that the carbon powder is better and uniformly dispersed in a resin matrix to form a more stable and compact network structure, improve the densification effect and improve the density of the carbon fiber composite material; and the mechanical property of the carbon fiber composite material is obviously improved. The addition of the self-dispersing carbon powder further increases the interface bonding strength of the resin adhesive and the carbon fiber, and improves the interlaminar shear strength of the carbon fiber composite material; the whole graphite structure of the material is improved, and the heat-conducting property of the carbon fiber composite material is further effectively improved.
Therefore, the densification method of the carbon fiber preform has the advantages that the densification effect is more excellent, the treatment period is obviously reduced, the density of the treated carbon fiber composite material is effectively improved, the interlayer bonding condition is improved, and the mechanical property is obviously enhanced; meanwhile, the heat-conducting property of the carbon fiber composite material is obviously improved.
Drawings
FIG. 1 is an IR spectrum of the surface-treated carbon powder and the self-dispersed carbon powder prepared in example 7 of the present invention.
Detailed Description
The technical solution of the present invention is further described in detail below with reference to the following detailed description and the accompanying drawings:
in the examples of the present invention, the phenolic resin used for the immersion treatment was PF9501, had a solid content of 82.4%, free phenol of 14.46%, a water content of 3.72%, a viscosity (25 ℃) of 5400 mPas, and a pH of 7.90. The phenolic resin used for the liquid phase impregnation treatment was PF9701, the solid content was 63.1%, the free phenol was 15.71%, the water content was 1.96%, and the viscosity (25 ℃ C.) was 110 mPas. Are all commercially available.
The preparation method of the carbon fiber preform used in the embodiment of the invention comprises the following steps:
s1: chopping 12K-specification carbon fiber tows to obtain 6cm chopped fiber carbon fibers, scattering, carding, net laying and needling, wherein the needling process is carried out by a flat needling machine, and special functional felting needles with barbs on edges are adopted for needling to prepare the chopped fiber carbon fibers with the gram weight of 90g/m2The net tire of (1);
s2: uniformly paving carbon fiber tows with the specification of 12K on the surface of a net tire by a mechanical method (single-layer one-way paving), then covering a layer of net tire on the surface of the paved and aged carbon fiber tows, introducing Z-direction fibers by a flat needle machine, combining the two layers of net tires, covering the fiber bundles in the net tires, and compounding by needling to obtain a prefabricated unit layer;
s3: continuously repeating the operation of the step S2 on the prefabricated unit layer until the designed thickness is reached to obtain the carbon fiber prefabricated body with the density of 0.5g/cm3。
Example 1:
a method of densifying a carbon fiber preform, comprising: firstly, carrying out soaking treatment, hot-pressing curing and carbonization treatment on a carbon fiber preform to obtain a carbon-carbon plate, and then carrying out liquid-phase impregnation treatment and carbonization treatment;
before liquid phase dipping treatment, the carbon fiber preform is pretreated, and the specific operations comprise:
dissolving dopamine in a Tris solution (pH 8.5) with the concentration of 10mM to obtain a dopamine solution with the concentration of 2.6mg/mL, adding iminodiacetic acid (the addition amount is 5 mg/mL), then soaking the dopamine solution in a carbon fiber preform, taking out the dopamine after soaking for 28 hours, and draining to obtain a pretreated carbon fiber preform;
the soaking treatment comprises the steps of soaking the pretreated carbon fiber preform in a resin adhesive composite liquid raw material for 5 hours;
the hot-pressing curing process comprises the following steps: under the condition of 8MPa pressure, the temperature is increased from 80 ℃ to 150 ℃ at the temperature increase rate of 5 ℃/min, and the temperature is naturally cooled to 80 ℃ after 6 hours of heat preservation.
The liquid phase impregnation treatment comprises: embedding a carbon-carbon plate by using a resin glue solution (prepared by adding 75% ethanol into phenolic resin according to the mass ratio of 1: 4), and setting the pressure to be 2MPa, the temperature to be 40 ℃ and the time to be 2h under the vacuum condition; then heating to 200 ℃ at the heating rate of 40 ℃/h, and curing for 2.5 h; and then naturally cooling to room temperature.
The carbonization treatment process comprises the following steps: under the protection of nitrogen gas, heating the temperature from 25 ℃ to 850 ℃ at the heating rate of 25 ℃/h, and keeping the constant temperature for 3 h; then raising the temperature to 1000 ℃ at the heating rate of 45 ℃/h, and keeping the temperature for 3 h; then cooling to 600 ℃ at a cooling rate of 50 ℃/h; then cooling to 300 ℃ at the cooling rate of 30 ℃/h, and then naturally cooling to below 100 ℃.
Taking liquid phase impregnation treatment and carbonization treatment as a complete treatment cycle, starting the next treatment cycle after carbonization treatment in the carbonization step, impregnating again in the impregnation step, and repeatedly treating for 5 times in this way;
the raw materials of the resin adhesive composite liquid comprise, by weight, 7 parts of resin adhesive, 40 parts of 75% ethanol, 10 parts of filler, 3 parts of carbon powder and 1.2 parts of p-toluenesulfonic acid. Wherein the resin adhesive is phenolic resin; the filler comprises wollastonite powder, black talcum powder, diatomite and barium sulfate, and the mass ratio of the wollastonite powder to the black talcum powder to the diatomite is 0.8:0.6:1: 0.6.
Example 2:
a densification method of a carbon fiber preform differs from that of example 1 in that:
in the pretreatment process of the carbon fiber preform, the concentration of the dopamine solution is 2.1mg/mL, and the addition amount of iminodiacetic acid is 5.5 mg/mL;
liquid-phase impregnation treatment process: the pressure is 3MPa, the temperature is 50 ℃, and the time is 1.5 h; then heating to 190 ℃ at the heating rate of 45 ℃/h, and curing for 3 h; and then naturally cooling to room temperature.
The raw materials of the resin adhesive composite liquid comprise, by weight, 5 parts of resin adhesive, 34 parts of 80% ethanol, 13 parts of filler, 4 parts of carbon powder and 1 part of p-toluenesulfonic acid. Wherein the resin glue is furan resin; the filler comprises wollastonite powder, black talcum powder, diatomite and barium sulfate, and the mass ratio of the wollastonite powder to the black talcum powder to the diatomite is 1:0.5:1: 0.7.
The liquid phase impregnation treatment and carbonization treatment were performed for the same number of treatment cycles as in example 1.
Example 3:
a densification method of a carbon fiber preform differs from that of example 1 in that:
in the pretreatment process of the carbon fiber preform, the concentration of the dopamine solution is 3mg/mL, and the addition amount of iminodiacetic acid is 6 mg/mL;
the raw materials of the resin adhesive composite liquid comprise, by weight, 9 parts of resin adhesive, 50 parts of 65% ethanol, 7 parts of filler, 2 parts of carbon powder and 1.5 parts of p-toluenesulfonic acid. Wherein the resin adhesive is phenolic resin; the filler comprises black talcum powder, diatomite and barium sulfate, and the mass ratio of the black talcum powder to the diatomite is 0.42:1: 0.68.
The liquid phase impregnation treatment and carbonization treatment were performed for the same number of treatment cycles as in example 1.
Example 4:
a densification method of a carbon fiber preform differs from that of example 1 in that:
in the pretreatment process of the carbon fiber preform, the concentration of the dopamine solution is 2.7mg/mL, and the addition amount of iminodiacetic acid is 5.8 mg/mL;
the raw materials of the resin adhesive composite liquid comprise, by weight, 8 parts of resin adhesive, 30 parts of 60% ethanol, 6 parts of filler, 5 parts of carbon powder and 0.8 part of p-toluenesulfonic acid. Wherein the resin adhesive is phenolic resin; the filler comprises wollastonite powder, diatomite and barium sulfate, and the mass ratio of the wollastonite powder to the diatomite is 0.9:1: 0.5.
The liquid phase impregnation treatment and carbonization treatment were performed for the same number of treatment cycles as in example 1.
Example 5:
a densification method of a carbon fiber preform differs from that of example 1 in that:
iminodiacetic acid is not added in the pretreatment process of the carbon fiber preform.
The liquid phase impregnation treatment and carbonization treatment were performed for the same number of treatment cycles as in example 1.
Example 6:
a densification method of a carbon fiber preform differs from example 1 in that:
the carbon fiber preform was not pretreated.
The liquid phase impregnation treatment and carbonization treatment were carried out for the same number of treatment cycles as in example 1.
Example 7:
a densification method of a carbon fiber preform differs from that of example 1 in that:
in the raw materials of the resin adhesive composite liquid, self-dispersing carbon powder is adopted to replace carbon powder;
preparation of the self-dispersing carbon powder:
dissolving KH550 and ammonia water in a mass ratio of 1:0.18 in a 90% ethanol solution (the mass ratio of KH550 to ethanol solution is 1: 40), adding carbon powder (the mass ratio of KH550 to KH550 is 1: 0.55), performing ultrasonic treatment for 35min, stirring at 40 deg.C for 22h, centrifuging, washing with ethanol for 5 times, drying at 60 deg.C for 10h, and grinding to obtain surface-treated carbon powder;
dissolving 5-chloropyridine-2-boronic acid pinacol ester in acetone at the concentration of 0.04g/mL, adding surface-treated carbon powder (the mass ratio of the surface-treated carbon powder to the 5-chloropyridine-2-boronic acid pinacol ester is 1: 1.2), adjusting the pH to 5.8 by using 1.4M sodium carbonate, stirring for 3 hours at the temperature of 40 ℃, centrifuging, washing the mixture solution of methanol and ethanol (v/v, 1: 1) for 5 times by centrifugation, and drying the mixture solution at the temperature of 55 ℃ to obtain the self-dispersing carbon powder.
The liquid phase impregnation treatment and carbonization treatment were performed for the same number of treatment cycles as in example 1.
Example 8:
a densification method of a carbon fiber preform differs from example 5 in that:
in the raw materials of the resin adhesive composite liquid, self-dispersing carbon powder is adopted to replace carbon powder;
the preparation of the self-dispersing carbon powder was the same as in example 7.
The liquid phase impregnation treatment and carbonization treatment were performed for the same number of treatment cycles as in example 1.
Example 9:
a densification method of a carbon fiber preform differs from example 6 in that:
in the raw materials of the resin adhesive composite liquid, self-dispersing carbon powder is adopted to replace carbon powder;
the preparation of the self-dispersing carbon powder was the same as in example 7.
The liquid phase impregnation treatment and carbonization treatment were performed for the same number of treatment cycles as in example 1.
Test example 1:
infrared testing
The test adopts a potassium bromide tabletting method and a Fourier infrared spectrometer for measurement. Wherein the wave number is 4000-500 cm-1。
The above tests were performed on the surface treated carbon powder of example 7 and the prepared self-dispersed carbon powder, and the results are shown in fig. 1. As can be seen from the analysis of the figure, 1635cm is found in the infrared spectrum of the surface-treated carbon powder-1The characteristic absorption peak of amino group in KH550 is close to the characteristic absorption peak, 1108cm-1The vicinity is a characteristic absorption peak of an O-Si bond in KH550, which indicates that the silane coupling agent is successfully introduced into the surface of the carbon powder. 1529cm in the infrared spectrum of the prepared self-dispersed carbon powder-1The characteristic absorption peak of imino group appears nearby, 1500-1400 cm-1The range of 1394cm shows a vibration absorption peak of benzene ring skeleton-1The characteristic absorption peak of B-O bond appears nearby, and the result shows that the self-dispersing carbon powder is successfully prepared.
Preparation and density measurement of carbon fiber composite material
And (3) sintering the densified carbon fiber preform at high temperature to prepare the carbon fiber composite material. Wherein, the high-temperature sintering process comprises the following steps: under the vacuum condition, gradually heating from room temperature to 1900 ℃ at the heating rate of 60 ℃/h, and preserving heat for 5h for sintering and purifying; then naturally cooling to 950 ℃, and then cooling to room temperature at a cooling rate of 40 ℃/h.
Density measurements were made using the Archimedes method.
The results of the above tests on carbon fiber preforms treated by the densification methods provided in examples 1 to 9 are shown in table 1:
table 1 Density test results
| Sample (I) | Density (g/cm)3） |
| Example 1 | 1.64 |
| Example 2 | 1.61 |
| Example 3 | 1.57 |
| Example 4 | 1.58 |
| Example 5 | 1.41 |
| Example 6 | 1.22 |
| Example 7 | 1.75 |
| Example 8 | 1.54 |
| Example 9 | 1.37 |
As can be seen from the analysis in table 1, after the carbon fiber preform is treated by the densification method provided in example 1, the density of the prepared carbon fiber composite material is significantly higher than that of example 5, the effect of example 5 is better than that of example 6, and the effects of examples 2 to 4 are equivalent to those of example 1, which indicates that the overall density of the carbon fiber composite material can be improved by performing the dipping pretreatment on the carbon fiber preform by using the dopamine solution; and iminodiacetic acid is added into the dopamine solution, so that the density of the carbon fiber composite material can be further improved. The effect of example 7 is better than that of example 1, the effect of example 8 is better than that of example 5, and the effect of example 9 is better than that of example 6, which shows that the self-dispersed carbon powder prepared by chemically treating the surface of the carbon powder with the silane coupling agent and the 5-chloropyridine-2-boronic acid pinacol ester can be applied to the densification treatment of the carbon fiber preform to further enhance the density of the carbon fiber composite material.
Test example 2:
interlaminar shear strength test
The test method is carried out according to the standard specified in GB 3357.
The carbon fiber composite materials prepared by sintering the densified preforms of examples 1 to 9 at high temperature were tested as described above, and the results are shown in table 2:
TABLE 2 interlaminar shear Strength test results
| Sample(s) | Interlaminar shear strength/MPa |
| Example 1 | 36.1 |
| Example 2 | 35.6 |
| Example 3 | 33.9 |
| Example 4 | 33.2 |
| Example 5 | 26.7 |
| Example 6 | 21.4 |
| Example 7 | 42.0 |
| Example 8 | 30.6 |
| Example 9 | 24.9 |
As can be seen from the analysis in table 2, after the carbon fiber preform is treated by the densification method provided in example 1, the interlaminar shear strength of the prepared carbon fiber composite material is significantly higher than that of example 5, the effect of example 5 is better than that of example 6, and the effects of examples 2 to 4 are equivalent to those of example 1, which indicates that the interlaminar adhesive property of the carbon fiber composite material can be improved by performing the dipping pretreatment on the carbon fiber preform by using the dopamine solution; and iminodiacetic acid is added into the dopamine solution, so that the interlaminar shear strength of the carbon fiber composite material can be further enhanced, and the interlaminar bonding performance of the composite material is improved. The effect of example 7 is better than that of example 1, the effect of example 8 is better than that of example 5, and the effect of example 9 is better than that of example 6, which shows that the self-dispersed carbon powder prepared by chemically treating the surface of carbon powder with a silane coupling agent and 5-chloropyridine-2-boronic acid pinacol ester can be applied to densification of a carbon fiber preform to further enhance the interlayer bonding capability of a carbon fiber composite material.
Test example 3:
test of compression resistance
The tests were carried out according to the standards specified in ASTM C695. The test specimens were processed into small cylinders of phi 10X 16mm and the parallel orientation was determined.
The carbon fiber composite materials obtained by sintering the densified preforms of examples 1 to 9 at high temperature were tested as described above, and the results are shown in table 3:
TABLE 3 compression resistance test results
| Sample (I) | Compressive strength/MPa |
| Example 1 | 204 |
| Example 2 | 200 |
| Example 3 | 195 |
| Example 4 | 192 |
| Example 5 | 171 |
| Example 6 | 156 |
| Example 7 | 236 |
| Example 8 | 201 |
| Example 9 | 174 |
As can be seen from the analysis in table 3, after the carbon fiber preform is treated by the densification method provided in example 1, the compressive strength of the prepared carbon fiber composite material in the parallel direction is significantly higher than that of example 5, the effect of example 5 is better than that of example 6, and the effects of examples 2 to 4 are equivalent to those of example 1, which indicates that the mechanical properties of the carbon fiber composite material can be improved by performing the dipping pretreatment on the carbon fiber preform by using the dopamine solution; and iminodiacetic acid is added into the dopamine solution, so that the compression resistance of the carbon fiber composite material can be further enhanced, and the mechanical property of the composite material is improved. The effect of example 7 is better than that of example 1, the effect of example 8 is better than that of example 5, and the effect of example 9 is better than that of example 6, which shows that the self-dispersed carbon powder prepared by chemically treating the surface of carbon powder with a silane coupling agent and 5-chloropyridine-2-boronic acid pinacol ester can be applied to the densification treatment of a carbon fiber preform to further enhance the pressure resistance of a carbon fiber composite material.
Test example 4:
test of Heat conductivity
The thermal conductivity of the samples was tested using an IR-2 laser thermal conductivity meter. The test specimens were processed to a specification of phi 10 × 16mm, and the test vertical direction (the direction in which the heat conduction is perpendicular to the rubbing surface is referred to as vertical).
The carbon fiber composite materials obtained by sintering the densified preforms of examples 1 to 9 at high temperature were tested as described above, and the results are shown in table 4:
TABLE 4 Heat transfer Performance test results
| Sample(s) | Coefficient of thermal conductivity (W/m. k) |
| Example 1 | 36.33 |
| Example 2 | 36.12 |
| Example 3 | 35.96 |
| Example 4 | 35.88 |
| Example 5 | 36.07 |
| Example 6 | 35.84 |
| Example 7 | 44.35 |
| Example 8 | 44.11 |
| Example 9 | 43.86 |
As can be seen from the analysis in table 4, after the carbon fiber preform is treated by the densification method provided in example 1, the thermal conductivity of the prepared carbon fiber composite material is equivalent to that of example 5, the effect of example 5 is equivalent to that of example 6, and the effects of examples 2 to 4 are equivalent to that of example 1, which indicates that the heat conductivity of the prepared carbon fiber composite material is not negatively affected by the impregnation pretreatment of the carbon fiber preform by using the dopamine solution; and the iminodiacetic acid is added into the dopamine solution, so that the heat conduction capability of the carbon fiber composite material is not negatively influenced. The effect of example 7 is better than that of example 1, the effect of example 8 is better than that of example 5, and the effect of example 9 is better than that of example 6, which shows that the silane coupling agent and 5-chloropyridine-2-boronic acid pinacol ester are used for carrying out chemical treatment on the surface of carbon powder to prepare the self-dispersed carbon powder, and the self-dispersed carbon powder is applied to densification of the carbon fiber preform, so that the thermal conductivity of the prepared carbon fiber composite material is obviously increased, and the thermal conductivity of the carbon fiber composite material is further enhanced.
Conventional techniques in the above embodiments are known to those skilled in the art, and therefore, will not be described in detail herein.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (9)
1. A method of densifying a carbon fiber preform, comprising: firstly, carrying out soaking treatment, hot-pressing curing and carbonization treatment on a carbon fiber preform to obtain a carbon-carbon plate, and then carrying out liquid-phase dipping treatment and carbonization treatment;
the soaking solution used in the soaking treatment process comprises a resin adhesive compound solution; the raw materials of the resin adhesive composite liquid comprise a resin adhesive, a diluent, a filler and carbon powder; the filler comprises at least one of wollastonite powder and black talcum powder, diatomite and barium sulfate; the impregnant used in the liquid phase impregnation treatment process comprises resin glue solution which consists of resin glue and a diluent;
the method is characterized in that: the carbon fiber preform is subjected to dipping treatment by using a dopamine solution containing iminodiacetic acid before the dipping treatment.
2. A method for densifying a carbon fiber preform according to claim 1, characterized in that: the resin adhesive comprises one of phenolic resin, epoxy resin and furan resin.
3. A method for densifying a carbon fiber preform according to claim 1, characterized in that: the diluent comprises 60-80% ethanol.
4. A method for densifying a carbon fiber preform according to claim 1, characterized in that: the carbon powder is in a nanometer level.
5. A method for densifying a carbon fiber preform according to claim 1, characterized in that: the resin adhesive composite liquid comprises, by weight, 4-10 parts of a resin adhesive, 20-60 parts of a diluent, 6-15 parts of a filler and 1-5 parts of carbon powder.
6. A method for densifying a carbon fiber preform according to claim 1, characterized in that: the addition amount of the iminodiacetic acid is 4-6 mg/mL.
7. A method for densifying a carbon fiber preform according to claim 1, characterized in that: the conditions of the liquid phase impregnation treatment include: the temperature is 30-50 ℃, and the dipping time is 1.5-3 h; then heating to 180-220 ℃ at a heating rate of 35-45 ℃/h, and curing for 2-4 h; then naturally cooling.
8. A method for densifying a carbon fiber preform according to claim 1, characterized in that: the mass ratio of resin glue to diluent in the resin glue solution is 1:3 to 5.
9. A method for densifying a carbon fiber preform according to claim 1, characterized in that: the filler comprises wollastonite powder, black talcum powder, diatomite and barium sulfate; the mass ratio of the wollastonite powder to the black talcum powder to the diatomite to the barium sulfate is 0.6-1: 0.4-0.8: 1: 0.5-0.7.
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