CN113172793A - Carbon-glass hybrid composite material curing process - Google Patents
Carbon-glass hybrid composite material curing process Download PDFInfo
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- CN113172793A CN113172793A CN202010571008.9A CN202010571008A CN113172793A CN 113172793 A CN113172793 A CN 113172793A CN 202010571008 A CN202010571008 A CN 202010571008A CN 113172793 A CN113172793 A CN 113172793A
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- 238000000034 method Methods 0.000 title claims abstract description 29
- 230000008569 process Effects 0.000 title claims abstract description 28
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 239000011521 glass Substances 0.000 title claims abstract description 24
- 239000003365 glass fiber Substances 0.000 claims abstract description 63
- 239000004917 carbon fiber Substances 0.000 claims abstract description 57
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 56
- 239000000835 fiber Substances 0.000 claims abstract description 54
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 39
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000010992 reflux Methods 0.000 claims abstract description 30
- 230000004048 modification Effects 0.000 claims abstract description 24
- 238000012986 modification Methods 0.000 claims abstract description 24
- 238000005406 washing Methods 0.000 claims abstract description 16
- 239000000853 adhesive Substances 0.000 claims abstract description 15
- 230000001070 adhesive effect Effects 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 238000009835 boiling Methods 0.000 claims abstract description 11
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 11
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 7
- 238000013329 compounding Methods 0.000 claims abstract description 6
- 238000005520 cutting process Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 24
- 238000002791 soaking Methods 0.000 claims description 20
- 238000003851 corona treatment Methods 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical class O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 16
- 229910052799 carbon Inorganic materials 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- 238000009832 plasma treatment Methods 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 239000003822 epoxy resin Substances 0.000 claims description 9
- 229920000647 polyepoxide Polymers 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000010884 ion-beam technique Methods 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 5
- 239000004593 Epoxy Substances 0.000 claims description 5
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 230000001678 irradiating effect Effects 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 11
- 239000007822 coupling agent Substances 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 238000004804 winding Methods 0.000 description 5
- -1 rare earth lanthanum chloride Chemical class 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000013081 microcrystal Substances 0.000 description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 235000019738 Limestone Nutrition 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052903 pyrophyllite Inorganic materials 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B11/00—Making preforms
- B29B11/14—Making preforms characterised by structure or composition
- B29B11/16—Making preforms characterised by structure or composition comprising fillers or reinforcement
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B11/00—Making preforms
- B29B11/06—Making preforms by moulding the material
Abstract
The invention discloses a carbon-glass hybrid composite material curing process, which comprises the following steps: firstly, modifying carbon fibers and glass fibers at one time: respectively carrying out short cutting treatment on the glass fiber and the carbon fiber until the length is 100-200mm, then compounding according to the weight ratio of 1:1, then carrying out pretreatment, then placing in a Soxhlet extractor, and washing the pretreated fiber by acetone solution in a refluxing manner. According to the invention, the carbon fiber and the glass fiber are subjected to primary modification, secondary modification and final modification, the activity of the fiber obtained through continuous modification treatment can be obviously improved, the fiber is subjected to boiling treatment of a rare earth solution in the primary modification, the surface structure becomes sparse, the coupling agent is easier to combine with the surface structure of the fiber in the secondary treatment, the treatment effect of the coupling agent is improved, and the combination strength of the fiber, a curing agent and a subsequent adhesive is enhanced.
Description
Technical Field
The invention relates to the technical field of carbon/glass fiber materials, in particular to a carbon-glass hybrid composite material curing process.
Background
The carbon fiber is a novel fiber material of high-strength and high-modulus fiber with the carbon content of more than 95 percent. It is made up by stacking organic fibres of flake graphite microcrystals along the axial direction of fibre, and making carbonization and graphitization treatment so as to obtain the invented microcrystal graphite material. The aluminum alloy is lighter than metal aluminum in mass, but higher than steel in strength, has the characteristics of corrosion resistance and high modulus, and is an important material in the aspects of national defense, military industry and civil use. It not only has the intrinsic characteristic of carbon material, but also has the soft workability of textile fiber, and is a new generation of reinforced fiber. The glass fiber is an inorganic non-metallic material with excellent performance, has various varieties, has the advantages of good insulativity, strong heat resistance, good corrosion resistance and high mechanical strength, but has the defects of brittleness and poor wear resistance. It is made up by using seven kinds of minerals of pyrophyllite, quartz sand, limestone, dolomite, borocalcite and boromagnesite as raw material through the processes of high-temp. melting, wire-drawing, winding and weaving, its monofilament diameter is several micrometers to twenty-several micrometers, and every fibre raw filament bundle is formed from hundreds of monofilaments, even thousands of monofilaments. Glass fibers are commonly used as reinforcing materials in composite materials, electrical and thermal insulation materials, circuit substrates, and other various fields of the national economy.
The existing carbon fiber and glass fiber have poor surface activity and poor reaction effect with a curing agent, so that the curing and forming effect is poor, and further improvement treatment is still needed.
The prior Chinese patent document publication No. CN109454893A discloses a novel carbon fiber tube processing technology, which comprises a solution preparation technology, a solution immersion technology, a winding forming technology and a curing technology, and is characterized in that: the carbon fiber tube processing technology comprises the following specific steps: s1, placing the prepared solution in a container; s2, soaking the carbon fiber composite material into the prepared solution to enable the surface of the material to be completely dipped with the solution; s3, winding the carbon fiber composite material dipped with the solution on a winding mold core, and forming the carbon fiber composite material by rotating the winding mold core; s4, curing the formed carbon fiber composite material in a curing furnace, wherein in the curing process, the curing furnace is firstly cured for one hour at a constant temperature of 150 ℃, then the curing furnace is cooled to room temperature, and simultaneously the curing furnace is cured for one hour again in a vacuum state formed by a vacuum pump, so that the solvent is thoroughly removed, and the strength of the formed carbon fiber is prevented from being influenced.
Disclosure of Invention
The invention aims to provide a carbon-glass hybrid composite material curing process to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme:
a carbon glass hybrid composite material curing process comprises the following steps:
firstly, modifying carbon fibers and glass fibers at one time: respectively carrying out short cutting treatment on glass fiber and carbon fiber until the length is 100-200mm, then compounding according to the weight ratio of 1:1, then carrying out pretreatment, then placing in a Soxhlet extractor, and washing the pretreated fiber by acetone solution in a refluxing manner;
secondly, secondary modification of carbon fibers and glass fibers: placing the primarily modified fiber in a reflux device, soaking the fiber in acetone, refluxing for 24h, wherein the heating temperature is 50-60 ℃, repeatedly soaking and washing the fiber in acetone for 3 times after the reaction is finished, carrying out ultrasonic treatment for 10-20min after each soaking, then placing the fiber in an oven for drying at the drying temperature of 80 ℃, then carrying out thermal reflux treatment on the fiber, and finally repeatedly washing the fiber with boiling water;
step three, final modification of carbon fiber and glass fiber: irradiating the carbon fiber and the glass fiber treated in the step two by adopting ion beam current of 2000pA, then performing corona treatment, placing the carbon fiber and the glass fiber in a glass container of aqueous solution after the corona treatment is finished, placing the carbon fiber and the glass fiber between an upper electrode and a lower electrode, opening a gas passage, and performing low-temperature plasma treatment;
step four, preparation of the adhesive curing agent: adding epoxy resin into organic modified silica sol according to the weight ratio of 1:2, firstly raising the temperature to 90 ℃, then stirring at the rotating speed of 100-;
step five, curing the carbon glass fiber: and (3) feeding the carbon fiber and the glass fiber in the third step and the adhesive curing agent in the fourth step into a high-temperature reaction kettle, mixing for 1-2h at the rotation speed of 100-300r/min at the temperature of 140-150 ℃ under the pressure of 5-10MPa, and then feeding into a mold for curing treatment, and finishing curing.
Preferably, the pretreatment in the first step is carried out by boiling the rare earth solution with rare earth lanthanum chloride as solute for 1-2h, wherein the boiling temperature is 100 ℃.
Preferably, the second step of thermal reflux treatment is to soak and reflux 5 mass percent of gamma-aminopropyltriethoxysilane and 3 mass percent of epoxy silane coupling agent KH-560 respectively, the heating temperature is 90-100 ℃, and the reflux time is 1-2 h.
Preferably, the corona treatment power in the third step is 2-6Kw, the treatment temperature is-10-20 ℃, and the treatment time is 10-20 min.
Preferably, the corona treatment power in the third step is 4Kw, the treatment temperature is 5 ℃, and the treatment time is 15 min.
Preferably, in the third step of low-temperature plasma treatment, the nitrogen flow is firstly adjusted to be 1-5L/min, the treatment time is 10-14s, a high-voltage power supply is started, and the voltage is controlled to be 8-12 KV.
Preferably, in the low-temperature plasma treatment, the nitrogen flow is firstly adjusted to be 3L/min, the treatment time is 12s, the high-voltage power supply is started, and the control voltage is 10 KV.
Preferably, the preparation method of the organic modified silica sol comprises the steps of adding the nano-silica into the organic silicon solution, stirring at a high speed of 2000r/min for 20-30min at 1000-.
Preferably, in the step five, the curing pressure in the curing treatment is 2-8MPa, the curing temperature is 60-100 ℃, and the demolding curing time is 2-10 h.
Preferably, the curing pressure in the curing treatment in the fifth step is 5MPa, the curing temperature is 80 ℃, and the demolding curing time is 6 h.
Compared with the prior art, the invention has the following beneficial effects:
(1) the carbon fiber and the glass fiber are subjected to primary modification, secondary modification and final modification, the activity of the fiber obtained by continuous modification treatment can be obviously improved, the fiber in the primary modification is subjected to boiling treatment of rare earth solution, the surface structure becomes sparse, the coupling agent in the secondary treatment is easier to combine with the surface structure of the fiber, the treatment effect of the coupling agent is improved, the bonding strength between the fiber and a curing agent and a subsequent adhesive is enhanced, the fiber is subjected to final treatment on the basis of the primary modification and the secondary modification, the final treatment is continuously performed by adopting ion beam, corona and plasma treatment, on one hand, the outer layer structure of the fiber treated by the coupling agent in the secondary modification is completely exposed, so that the outer layer structure is combined with the curing agent to a greater extent, on the other hand, the contact angle of the fiber is improved, so that the mechanical property between the glass fiber and the carbon fiber is improved, and the fiber is combined with the curing agent to form a net structure in the curing process more conveniently and rapidly, the firm structure of formation integral type has very big improvement the solidification effect.
(2) After the epoxy resin is treated by the organic modified silica sol, the silicon dioxide is attached to the surface of the epoxy resin, and the silicon dioxide has strong activity and high specific surface area and is treated by the organic silicon solution, so that the contact effect of the epoxy resin and the hybrid fiber can be improved, and the curing effect is improved.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the carbon-glass hybrid composite material curing process of the embodiment comprises the following steps:
firstly, modifying carbon fibers and glass fibers at one time: respectively carrying out short cutting treatment on glass fibers and carbon fibers until the length is 100mm, then compounding according to the weight ratio of 1:1, then carrying out pretreatment, then placing in a Soxhlet extractor, and washing the pretreated fibers by acetone solution in a refluxing manner;
secondly, secondary modification of carbon fibers and glass fibers: placing the primarily modified fiber in a reflux device, soaking the fiber in acetone, refluxing for 24h, heating to 50 ℃, repeatedly soaking and washing the fiber in acetone for 3 times after the reaction is finished, carrying out ultrasonic treatment for 10min after each soaking, then placing the fiber in an oven for drying at the drying temperature of 80 ℃, then carrying out thermal reflux treatment on the fiber, and finally repeatedly washing the fiber with boiling water;
step three, final modification of carbon fiber and glass fiber: irradiating the carbon fiber and the glass fiber treated in the step two by adopting ion beam current of 2000pA, then performing corona treatment, placing the carbon fiber and the glass fiber in a glass container of aqueous solution after the corona treatment is finished, placing the carbon fiber and the glass fiber between an upper electrode and a lower electrode, opening a gas passage, and performing low-temperature plasma treatment;
step four, preparation of the adhesive curing agent: adding epoxy resin into organic modified silica sol according to the weight ratio of 1:2, firstly heating to 90 ℃, then stirring at the rotating speed of 100r/min for 20min, then curing at 115 ℃ for 2-35min, and then cooling to obtain an adhesive;
step five, curing the carbon glass fiber: and (3) feeding the carbon fibers and the glass fibers in the third step and the adhesive curing agent in the fourth step into a high-temperature reaction kettle together, mixing for 1h at the rotating speed of 100r/min under the pressure of 5MPa and at the temperature of 140 ℃, then feeding into a mold for curing treatment, and finishing curing.
In the first step of this example, the rare earth solution with the rare earth lanthanum chloride as the solute was boiled for 1 hour at 100 ℃.
In the second step of the present embodiment, 5% by mass of γ -aminopropyltriethoxysilane and 3% by mass of an epoxy silane coupling agent KH-560 are respectively used for soaking and refluxing, the heating temperature is 90 ℃, and the refluxing time is 1 hour.
In the third step of this example, the corona treatment power was 2Kw, the treatment temperature was-10 deg.C, and the treatment time was 10 min.
In the third low-temperature plasma treatment in this embodiment, the nitrogen flow is first adjusted to 1L/min, the treatment time is 10s, the high-voltage power supply is started, and the control voltage is 8 KV.
The preparation method of the organic modified silica sol of the embodiment includes adding the nano-silica into the organic silicon solution, stirring at a high speed of 1000r/min for 20min, and then stirring at a low speed of 200r/min for 1h to obtain the modified silica sol.
In the fifth step of this example, the curing pressure in the curing process is 2MPa, the curing temperature is 60 ℃, and the demolding curing time is 2 hours.
Example 2:
the carbon-glass hybrid composite material curing process of the embodiment comprises the following steps:
firstly, modifying carbon fibers and glass fibers at one time: respectively carrying out short cutting treatment on glass fibers and carbon fibers until the length is 200mm, then compounding according to the weight ratio of 1:1, then carrying out pretreatment, then placing in a Soxhlet extractor, and washing the pretreated fibers by acetone solution in a refluxing manner;
secondly, secondary modification of carbon fibers and glass fibers: placing the primarily modified fiber in a reflux device, soaking the fiber in acetone, refluxing for 24h, heating to 60 ℃, repeatedly soaking and washing the fiber in acetone for 3 times after the reaction is finished, carrying out ultrasonic treatment for 20min after each soaking, then placing the fiber in an oven for drying at the drying temperature of 80 ℃, then carrying out thermal reflux treatment on the fiber, and finally repeatedly washing the fiber with boiling water;
step three, final modification of carbon fiber and glass fiber: irradiating the carbon fiber and the glass fiber treated in the step two by adopting ion beam current of 2000pA, then performing corona treatment, placing the carbon fiber and the glass fiber in a glass container of aqueous solution after the corona treatment is finished, placing the carbon fiber and the glass fiber between an upper electrode and a lower electrode, opening a gas passage, and performing low-temperature plasma treatment;
step four, preparation of the adhesive curing agent: adding epoxy resin into organic modified silica sol according to the weight ratio of 1:2, firstly heating to 90 ℃, then stirring at the rotating speed of 200r/min for 30min, then curing at 125 ℃ for 35min, and then cooling to obtain an adhesive;
step five, curing the carbon glass fiber: and (3) feeding the carbon fibers and the glass fibers in the third step and the adhesive curing agent in the fourth step into a high-temperature reaction kettle together, mixing for 2 hours at the rotating speed of 300r/min under the pressure of 10MPa and at the temperature of 150 ℃, then feeding into a mold for curing treatment, and finishing curing.
In the first step of this example, the rare earth solution with the rare earth lanthanum chloride as the solute was boiled for 2 hours at 100 ℃.
In the second step of the present embodiment, 5% by mass of γ -aminopropyltriethoxysilane and 3% by mass of an epoxy silane coupling agent KH-560 are respectively used for soaking and refluxing, the heating temperature is 100 ℃, and the refluxing time is 2 hours.
In the third step of this example, the corona treatment power was 6Kw, the treatment temperature was-20 deg.C, and the treatment time was 20 min.
In the third low-temperature plasma treatment in this embodiment, the nitrogen flow is first adjusted to 5L/min, the treatment time is 14s, the high-voltage power supply is started, and the control voltage is 12 KV.
The preparation method of the organic modified silica sol comprises the steps of adding the nano silicon dioxide into the organic silicon solution, stirring at a high speed of 2000r/min for 30min, and then stirring at a low speed of 300r/min for 2h to obtain the modified silica sol.
In the fifth step of this example, the curing pressure in the curing process is 8MPa, the curing temperature is 100 ℃, and the demolding curing time is 10 hours.
Example 3:
the carbon-glass hybrid composite material curing process of the embodiment comprises the following steps:
firstly, modifying carbon fibers and glass fibers at one time: respectively carrying out short cutting treatment on glass fibers and carbon fibers until the length is 150mm, then compounding according to the weight ratio of 1:1, then carrying out pretreatment, then placing in a Soxhlet extractor, and washing the pretreated fibers by acetone solution in a refluxing manner;
secondly, secondary modification of carbon fibers and glass fibers: placing the primarily modified fiber in a reflux device, soaking the fiber in acetone, refluxing for 24h, wherein the heating temperature is 55 ℃, repeatedly soaking and washing the fiber for 3 times after the reaction is finished, carrying out ultrasonic treatment for 15min after each soaking, then placing the fiber in an oven for drying at the drying temperature of 80 ℃, then carrying out thermal reflux treatment on the fiber, and finally repeatedly washing the fiber with boiling water;
step three, final modification of carbon fiber and glass fiber: irradiating the carbon fiber and the glass fiber treated in the step two by adopting ion beam current of 2000pA, then performing corona treatment, placing the carbon fiber and the glass fiber in a glass container of aqueous solution after the corona treatment is finished, placing the carbon fiber and the glass fiber between an upper electrode and a lower electrode, opening a gas passage, and performing low-temperature plasma treatment;
step four, preparation of the adhesive curing agent: adding epoxy resin into organic modified silica sol according to the weight ratio of 1:2, firstly heating to 90 ℃, then stirring at the rotating speed of 150r/min for 25min, then curing at 120 ℃ for 30min, and then cooling to obtain an adhesive;
step five, curing the carbon glass fiber: and (3) feeding the carbon fibers and the glass fibers in the third step and the adhesive curing agent in the fourth step into a high-temperature reaction kettle, mixing at the rotating speed of 200r/min for 1.5h at the temperature of 145 ℃ under 7.5MPa, and then feeding into a mold for curing treatment, wherein the curing is finished.
In the first step of this example, the rare earth solution with the rare earth lanthanum chloride as the solute is boiled for 1-2h at 100 ℃.
In the second step of the present embodiment, 5% by mass of γ -aminopropyltriethoxysilane and 3% by mass of an epoxy silane coupling agent KH-560 are respectively used for soaking and refluxing, the heating temperature is 100 ℃, and the refluxing time is 2 hours.
In the third step of this example, the corona treatment power was 6Kw, the treatment temperature was 20 ℃, and the treatment time was 20 min.
In the third low-temperature plasma treatment in this embodiment, the nitrogen flow is first adjusted to 5L/min, the treatment time is 14s, the high-voltage power supply is started, and the control voltage is 12 KV.
The preparation method of the organic modified silica sol comprises the steps of adding the nano silicon dioxide into the organic silicon solution, stirring at a high speed of 2000r/min for 30min, and then stirring at a low speed of 300r/min for 2h to obtain the modified silica sol.
In the fifth step of this example, the curing pressure in the curing process is 8MPa, the curing temperature is 100 ℃, and the demolding curing time is 10 hours.
Comparative example 1:
the material and preparation process are basically the same as those of example 3, except that the carbon fiber and the glass fiber are not subjected to final modification treatment.
Comparative example 2:
the materials and preparation process were substantially the same as those of example 3, except that the epoxy resin was not treated with the organic modified silica sol.
Comparative example 3:
basically the same materials and preparation process as those in example 3, except that the raw materials and method in example 1 in the novel carbon fiber tube processing process are compounded with glass fibers as disclosed in chinese patent publication No. CN 109454893A.
And (3) performance testing: the materials prepared in examples 1-3 and comparative examples 1-3 were tested for properties according to DB34/T5065-2016, and the results are shown in Table 1:
as can be seen from table 1, the bonding strength between carbon glass fibers in example 3 of the present invention can reach 6.2MPa, the bonding strength between carbon glass fibers in comparative example 3 is 2.1MPa, example 3 is 4.1MPa higher than comparative example 3, the tensile strength of carbon glass fibers in example 3 is 419MPa, the tensile strength of carbon glass fibers in comparative example 3 is 312MPa, and the tensile strength of carbon glass fibers in example 3 is 107MPa higher than comparative example 3, and the improvement rate is 34.29%, so that the bonding strength between carbon glass fibers and the tensile strength of carbon glass fibers in the curing process of the present invention are significantly improved.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. The carbon-glass hybrid composite material curing process is characterized by comprising the following steps of:
firstly, modifying carbon fibers and glass fibers at one time: respectively carrying out short cutting treatment on glass fiber and carbon fiber until the length is 100-200mm, then compounding according to the weight ratio of 1:1, then carrying out pretreatment, then placing in a Soxhlet extractor, and washing the pretreated fiber by acetone solution in a refluxing manner;
secondly, secondary modification of carbon fibers and glass fibers: placing the primarily modified fiber in a reflux device, soaking the fiber in acetone, refluxing for 24h, wherein the heating temperature is 50-60 ℃, repeatedly soaking and washing the fiber in acetone for 3 times after the reaction is finished, carrying out ultrasonic treatment for 10-20min after each soaking, then placing the fiber in an oven for drying at the drying temperature of 80 ℃, then carrying out thermal reflux treatment on the fiber, and finally repeatedly washing the fiber with boiling water;
step three, final modification of carbon fiber and glass fiber: irradiating the carbon fiber and the glass fiber treated in the step two by adopting ion beam current of 2000pA, then performing corona treatment, placing the carbon fiber and the glass fiber in a glass container of aqueous solution after the corona treatment is finished, placing the carbon fiber and the glass fiber between an upper electrode and a lower electrode, opening a gas passage, and performing low-temperature plasma treatment;
step four, preparation of the adhesive curing agent: adding epoxy resin into organic modified silica sol according to the weight ratio of 1:2, firstly raising the temperature to 90 ℃, then stirring at the rotating speed of 100-;
step five, curing the carbon glass fiber: and (3) feeding the carbon fiber and the glass fiber in the third step and the adhesive curing agent in the fourth step into a high-temperature reaction kettle, mixing for 1-2h at the rotation speed of 100-300r/min at the temperature of 140-150 ℃ under the pressure of 5-10MPa, and then feeding into a mold for curing treatment, and finishing curing.
2. The curing process of the carbon-glass hybrid composite material as claimed in claim 1, wherein the pretreatment in the first step is performed by boiling the rare earth solution with lanthanum chloride as a solute for 1-2h, wherein the boiling temperature is 100 ℃.
3. The curing process of the carbon-glass hybrid composite material as claimed in claim 1, wherein the second thermal reflow treatment step is performed by soaking and reflowing 5 mass percent of gamma-aminopropyltriethoxysilane and 3 mass percent of epoxy silane coupling agent KH-560 respectively, wherein the heating temperature is 90-100 ℃ and the reflowing time is 1-2 h.
4. The curing process of the carbon-glass hybrid composite material as claimed in claim 1, wherein the corona treatment power in the third step is 2-6Kw, the treatment temperature is-10-20 ℃, and the treatment time is 10-20 min.
5. The curing process of the carbon-glass hybrid composite material as claimed in claim 4, wherein the corona treatment power in the third step is 4Kw, the treatment temperature is 5 ℃, and the treatment time is 15 min.
6. The curing process of the carbon-glass hybrid composite material as claimed in claim 1, wherein in the third step of low temperature plasma treatment, the nitrogen flow is firstly adjusted to 1-5L/min, the treatment time is 10-14s, the high voltage power supply is started, and the control voltage is 8-12 KV.
7. The curing process of the carbon-glass hybrid composite material as claimed in claim 6, wherein in the low-temperature plasma treatment, the nitrogen flow is adjusted to 3L/min, the treatment time is 12s, the high-voltage power supply is started, and the control voltage is 10 KV.
8. The curing process of the carbon-glass hybrid composite material as claimed in claim 1, wherein the preparation method of the organic modified silica sol comprises adding the nano-silica into the organic silicon solution, stirring at a high speed of 1000-2000r/min for 20-30min, and then stirring at a low speed of 200-300r/min for 1-2h to obtain the modified silica sol.
9. The curing process of the carbon-glass hybrid composite material as claimed in claim 1, wherein in the step five, the curing pressure in the curing process is 2-8MPa, the curing temperature is 60-100 ℃, and the demolding curing time is 2-10 h.
10. The curing process of the carbon-glass hybrid composite material as claimed in claim 9, wherein the curing pressure in the curing treatment in the fifth step is 5MPa, the curing temperature is 80 ℃, and the demolding curing time is 6 hours.
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