CN106240126B - Polyborosiloxane-carbon fiber fabric swatch and its dissolving dipping hot pressing the preparation method - Google Patents
Polyborosiloxane-carbon fiber fabric swatch and its dissolving dipping hot pressing the preparation method Download PDFInfo
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- CN106240126B CN106240126B CN201610605586.3A CN201610605586A CN106240126B CN 106240126 B CN106240126 B CN 106240126B CN 201610605586 A CN201610605586 A CN 201610605586A CN 106240126 B CN106240126 B CN 106240126B
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- carbon cloth
- polyborosiloxane
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- composite plate
- dissolving
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/08—Impregnating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
- B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
- B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
- B32B2260/02—Composition of the impregnated, bonded or embedded layer
- B32B2260/021—Fibrous or filamentary layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
- B32B2260/04—Impregnation, embedding, or binder material
- B32B2260/046—Synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/10—Inorganic fibres
- B32B2262/106—Carbon fibres, e.g. graphite fibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/306—Resistant to heat
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
Abstract
The invention discloses polyborosiloxane carbon cloth composite plates and its dissolving dipping hot pressing the preparation method to pre-process carbon cloth using carbon cloth and polyborosiloxane performed polymer as raw material, prepares polyborosiloxane carbon cloth composite plate.In a solvent by the dissolving of polyborosiloxane performed polymer, maceration extract is made, pretreated carbon cloth will be passed through and immerse maceration extract 38 minutes, taken out after natural drying, be put into vacuum drying oven and dried 12 hours at 50 DEG C；By treated, carbon cloth stacks in a mold, and polyborosiloxane carbon cloth composite plate is obtained using accurate tablet press machine is hot-forming.The composite plate is not easy to be layered, and has preferable mechanical property and corrosion-resistant and high-temperature resistant performance, the feature that the present invention has preparation method simple, easily operated.
Description
Technical field
The present invention relates to field of high polymer composite material preparation, and in particular to a kind of polyborosiloxane-carbon cloth and its
Dissolving dipping hot pressing method for preparing.
Background technology
Carbon cloth is also known as carbon fiber woven cloth or carbon fiber reinforcement cloth, is used for tension, shearing resistance and the antidetonation of structural elements
It reinforces, which is used in conjunction with the carbon fiber that may make up complete performance brilliance as carbon fibre composite with mating dipping glue
Tie up cloth sheet material reinforcement system.
In numerous Behavior of Carbon Fiber Reinforced Polymer, carbon cloth enhancing polymer matrix composite it is light, than strong
Degree, specific stiffness and specific modulus are big, high temperature resistant, heat stabilizer are good, are widely used in the fields such as aerospace, military affairs, athletics sports,
It can be used for manufacturing fuselage, rudder, the engine shell of rocket, guided missile air diffuser, fishing rod, baseball rod, sledding, speedboat, feather
The high-grade fireproof garment of the special occupations such as the structural members such as racket and army, fire-fighting, steel mill.
As the development of composite technology and parts and structural member lightweight, high performance and functionalization chase after
It asks, using the component of carbon fiber reinforced polymers increasing, carbon fiber higher and higher using the ratio of carbon fiber reinforced polymers
The structure of dimension cloth composite element also becomes increasingly complex.China is concentrated mainly on epoxy to the research of carbon fiber reinforced polymers
In terms of resin-based materials.Peng Yongli etc. is using carbon cloth as reinforcing material, phenolic resin, and epoxy resin passes through as matrix
Dipping, the techniques such as laminated into type, carbon cloth, which is made, enhances composite material of novolac epoxy resin, when epoxy resin mass fraction is
When 25%, which has maximum bending strength 265MPa.But epoxies adhesive high temperature resistance is bad, with temperature
Degree increases, and the tensile shear strength of epoxies adhesive reduces rapidly, and 800When its tensile shear strength is only room temperature when C
37%, lead to its epoxies adhesive premature failure under open fire effect between carbon cloth and composite material surface.
Invention content
The present invention provides a kind of polyborosiloxane-carbon cloth composite plate and its dissolving dipping hot pressing regarding to the issue above
The preparation method.
The technical solution adopted by the present invention is：Polyborosiloxane-carbon cloth composite plate, by passing through pretreated carbon fiber
Cloth is stacked in mold, is obtained by hot-forming.
The dissolving of polyborosiloxane-carbon cloth composite plate impregnates hot pressing the preparation method, includes the following steps
The pretreatment of step 1 carbon cloth：Carbon cloth is cut into required size, is put into absolute ethyl alcohol and uses
Ultrasonic wave embathes 3-5 minutes, is put into after drying in Muffle furnace in 4500C is calcined 1 hour；
The preparation of step 2 maceration extract：In a solvent by the dissolving of polyborosiloxane performed polymer, solution temperature is room temperature-
800C is configured to the maceration extract of a concentration of 3-20g/L；
The preparation of step 3 hard board：Pretreated carbon cloth will be passed through and immerse maceration extract 3-8 minutes, nature is taken out and dry in the air
After dry, it is put into vacuum drying oven in 500It is dried 12 hours under C；Next the carbon cloth after drying is stacked according to required thickness
In a mold, polyborosiloxane-carbon cloth composite plate is obtained using accurate tablet press machine is hot-forming.
As a kind of perferred technical scheme：In polyborosiloxane-carbon cloth composite plate, the content of fiber is in 35%-
50%。
As a kind of perferred technical scheme：Carbon cloth is plain weave, twill or satin weave, the model of carbon cloth
1K, 3K, 6K or 12K, 200,240 or 300g/m of density3。
As a kind of perferred technical scheme：Carbon cloth includes two-dimentional carbon cloth and three-dimensional carbon cloth.
As a kind of perferred technical scheme：Polyborosiloxane performed polymer is poly- diphenyl Borosiloxane performed polymer, point
Son amount is 500-1000, the molar ratio 3 of silicon boron：1-1：1.
As a kind of perferred technical scheme：The solvent for preparing maceration extract can be dimethylbenzene, toluene, tetrahydrofuran, second
One or more of alcohol, N-Methyl pyrrolidone, dimethylformamide, pyridine.
As a kind of perferred technical scheme：Temperature is 260-300 when hot-forming using accurate tablet press machine0C, pressure are
6-9MPa, time are 7-15 minutes.
As a kind of perferred technical scheme：The carbon cloth layer structure thickness alternate with polyborosiloxane performed polymer is extremely
It is more than 1mm less.
The beneficial effects of the invention are as follows：Hot pressing the preparation method is impregnated using the dissolving of polyborosiloxane-carbon cloth composite plate
Composite plate obtained is not easy to be layered, and has preferable mechanical property and corrosion-resistant and high-temperature resistant performance；The present invention has preparation method
Simply, easily operated feature.
Description of the drawings
Fig. 1 show the surface scan electron microscope of polyborosiloxane-carbon cloth composite plate；
Fig. 2 show the scanning electron microscope (SEM) photograph after polyborosiloxane-carbon cloth composite plate tension failure.
Specific implementation mode
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is technology description to be briefly described, it is therefore apparent that drawings in the following description are only some embodiments of the invention.
Embodiment 1：
By 3K plain weaves, density 200g/m3Carbon cloth be cut into 60mm × 40mm sizes, it is super with absolute ethyl alcohol
Sound wave embathes 3 minutes, is put into after drying 450 in Muffle furnace0C is calcined 1 hour.Silicon boron in poly- diphenyl Borosiloxane performed polymer
Molar ratio 3：1, molecular weight 800.By poly- diphenyl Borosiloxane performed polymer in 800C is dissolved in dimethylbenzene, is configured to concentration
For the maceration extract of 10g/L.Pretreated carbon cloth will be passed through and immerse maceration extract 4 minutes, take out after natural drying, be put into vacuum
50 in baking oven0It is dried 12 hours under C；It waits for that mold coats die sinking agent, after carbon cloth is laminated to 3.1mm thickness, is put into mold,
It is hot-forming using accurate tablet press machine, temperature 2600C, pressure 8MPa, time are 10 minutes, obtain polyborosiloxane-carbon
Fiber cloth composite plate.In prepared carbon cloth composite plate, fiber content 40%, polyborosiloxane-carbon cloth of preparation
Composite plate tensile strength is 202MPa, elasticity modulus 862MPa.
Fig. 1 is the scanning electron microscope (SEM) photograph of 1 polyborosiloxane of embodiment-carbon cloth composite surface, and Fig. 2 is poly- borosilicate oxygen
Scanning electron microscope (SEM) photograph after alkane-carbon cloth composite plate tension failure.It is clear from fig. 1 that polyborosiloxane is substantially completely
It is impregnated into the latitude and longitude of carbon cloth, and together with carbon cloth tight bond, forms and spread all over different layers carbon cloth
All composite plates.Figure it is seen that intersecting and restraining between polyborosiloxane-carbon cloth composite plate fiber, it is broken
When be the fibrous fracture parallel with draw direction, the polyborosiloxane for playing cementation is broken powdering completely, so as to
Improve the intensity and anti-fatigue ability of material.
Embodiment 2：
By 3K plain weaves, density 240g/m3Carbon cloth be cut into 60mm × 40mm sizes, it is super with absolute ethyl alcohol
Sound wave embathes 4 minutes, is put into after drying 450 in Muffle furnace0C is calcined 1 hour.Silicon boron in poly- diphenyl Borosiloxane performed polymer
Molar ratio 3：1, molecular weight 700.By poly- diphenyl Borosiloxane performed polymer in 500C is dissolved in tetrahydrofuran, is configured to dense
Degree is the maceration extract of 15g/L.Pretreated carbon cloth will be passed through and immerse maceration extract 3 minutes, taken out after natural drying, be put into true
50 in empty baking oven0It is dried 12 hours under C；It waits for that mold coats die sinking agent, after carbon cloth is laminated to 2.2mm thickness, is put into mold
In, temperature 280 hot-forming using accurate tablet press machine0C, pressure 7MPa, time are 13 minutes, obtain polyborosiloxane-
Carbon cloth composite plate.In prepared carbon cloth composite plate, fiber content 41%, polyborosiloxane-carbon fiber of preparation
Cloth composite plate tensile strength is 189MPa, elasticity modulus 726MPa.
Embodiment 3：
By 12K plain weaves, density 300g/m3Carbon cloth be cut into 61mm × 40mm sizes, use absolute ethyl alcohol
Ultrasonic wave embathes 4 minutes, is put into after drying 450 in Muffle furnace0C is calcined 1 hour.Silicon boron in poly- diphenyl Borosiloxane performed polymer
Molar ratio 2：1, molecular weight 1000.By poly- diphenyl Borosiloxane performed polymer in room-temperature dissolution in absolute ethyl alcohol and dimethylbenzene
In mixed liquor（Dimethylbenzene and absolute ethyl alcohol volume ratio are 1:1）, it is configured to the maceration extract of a concentration of 3g/L.It will pass through pretreated
Carbon cloth immerses maceration extract 4 minutes, takes out after natural drying, is put into 50 in vacuum drying oven0It is dried 12 hours under C；Wait for that mold applies
Upper die sinking agent is put into after carbon cloth is laminated to 2.0mm thickness in mold, hot-forming using accurate tablet press machine, and temperature is
2900C, pressure 7MPa, time are 15 minutes, obtain polyborosiloxane-carbon cloth composite plate.Prepared carbon cloth
In composite plate, polyborosiloxane-carbon cloth composite plate tensile strength of fiber content 38%, preparation is 164MPa, springform
Amount is 607MPa.
Embodiment 4：
By 1K plain weaves, density 200g/m3Carbon cloth be cut into 58mm × 43mm sizes, it is super with absolute ethyl alcohol
Sound wave embathes 3 minutes, is put into after drying 450 in Muffle furnace0C is calcined 1 hour.Silicon boron in poly- diphenyl Borosiloxane performed polymer
Molar ratio 1：1, molecular weight 900.Poly- diphenyl Borosiloxane performed polymer is matched in room-temperature dissolution in N-Methyl pyrrolidone
The maceration extract of a concentration of 20g/L is made.Pretreated carbon cloth will be passed through and immerse maceration extract 3 minutes, taken out after natural drying,
It is put into 50 in vacuum drying oven0It is dried 12 hours under C；It waits for that mold coats die sinking agent, after carbon cloth is laminated to 2.9mm thickness, puts
Enter in mold, temperature 280 hot-forming using accurate tablet press machine0C, pressure 8MPa, time are 12 minutes, obtain poly- boron
Siloxanes-carbon cloth composite plate.In prepared carbon cloth composite plate, fiber content 42%, the poly- borosilicate oxygen of preparation
Alkane-carbon cloth composite plate tensile strength is 192MPa, elasticity modulus 801MPa.
Embodiment 5
By 6K plain weaves, density 200g/m3Carbon cloth be cut into 61mm × 40mm sizes, it is super with absolute ethyl alcohol
Sound wave embathes 3 minutes, is put into after drying 450 in Muffle furnace0C is calcined 1 hour.Silicon boron in poly- diphenyl Borosiloxane performed polymer
Molar ratio 3：1, molecular weight 800.Poly- diphenyl Borosiloxane performed polymer is configured to concentration in room-temperature dissolution in dimethylbenzene
For the maceration extract of 10g/L.Pretreated carbon cloth will be passed through and immerse maceration extract 4 minutes, take out after natural drying, be put into vacuum
50 in baking oven0It is dried 12 hours under C；It waits for that mold coats die sinking agent, after carbon cloth is laminated to 4.2mm thickness, is put into mold,
It is hot-forming using accurate tablet press machine, temperature 3000C, pressure 6MPa, time are 13 minutes, obtain polyborosiloxane-carbon
Fiber cloth composite plate.In prepared carbon cloth composite plate, fiber content 40%, polyborosiloxane-carbon cloth of preparation
Composite plate tensile strength is 225MPa, elasticity modulus 859MPa.
Embodiment 6
By 6K plain weaves, density 200g/m3Carbon cloth be cut into 58mm × 39mm sizes, it is super with absolute ethyl alcohol
Sound wave embathes 5 minutes, is put into after drying 450 in Muffle furnace0C is calcined 1 hour.Silicon boron in poly- diphenyl Borosiloxane performed polymer
Molar ratio 2：1, molecular weight 600.By poly- diphenyl Borosiloxane performed polymer in 800C is dissolved in dimethylbenzene, is configured to concentration
For the maceration extract of 15g/L.Pretreated carbon cloth will be passed through and immerse maceration extract 8 minutes, take out after natural drying, be put into vacuum
50 in baking oven0It is dried 12 hours under C；It waits for that mold coats die sinking agent, after carbon cloth is laminated to 5.0mm thickness, is put into mold,
It is hot-forming using accurate tablet press machine, temperature 3000C, pressure 9MPa, time are 7 minutes, obtain polyborosiloxane-carbon fiber
Tie up cloth composite plate.In prepared carbon cloth composite plate, polyborosiloxane-carbon cloth of fiber content 35%, preparation is multiple
Plywood tensile strength is 248MPa, elasticity modulus 945MPa.
It should be noted last that above example is only unrestricted to supplement explaination technical scheme of the present invention.To the greatest extent
Pipe is described the invention in detail with reference to embodiment, and this field vast is it will be appreciated by the skilled person that skill to the present invention
Art scheme is modified or is replaced on an equal basis, without departure from the spirit and scope of technical solution of the present invention, should all cover at this
In the right of invention.
Claims (5)
1. the dissolving of polyborosiloxane-carbon cloth composite plate impregnates hot pressing the preparation method, the polyborosiloxane-carbon cloth is compound
Plate is by being stacked in mold by pretreated carbon cloth, being obtained by hot-forming；Preparation method is characterized in that：
Include the following steps
The pretreatment of step 1 carbon cloth：It carbon cloth is cut into required size is put into absolute ethyl alcohol and use ultrasonic wave
It embathes 3-5 minutes, is put into after drying in Muffle furnace and is calcined 1 hour in 450 DEG C；
The preparation of step 2 maceration extract：In a solvent by the dissolving of polyborosiloxane performed polymer, solution temperature is -80 DEG C of room temperature, is matched
The maceration extract of a concentration of 3-20g/L is made；
The polyborosiloxane performed polymer be poly- diphenyl Borosiloxane performed polymer, molecular weight 500-1000, silicon boron
Molar ratio 3：1-1：1；
The solvent for preparing maceration extract can be dimethylbenzene, toluene, tetrahydrofuran, ethyl alcohol, N-Methyl pyrrolidone, dimethyl formyl
One or more of amine, pyridine；
The preparation of step 3 hard board：Pretreated carbon cloth will be passed through and immerse maceration extract 3-8 minutes, take out naturally dry
Afterwards, it is put into vacuum drying oven and is dried 12 hours at 50 DEG C；Next the carbon cloth after drying is overlayed according to required thickness
In mold, polyborosiloxane-carbon cloth composite plate is obtained using accurate tablet press machine is hot-forming；
Temperature is 260-300 DEG C, pressure 6-9MPa when hot-forming using accurate tablet press machine, and the time is 7-15 minutes.
2. the dissolving of polyborosiloxane according to claim 1-carbon cloth composite plate impregnates hot pressing the preparation method, feature
It is：In polyborosiloxane-carbon cloth composite plate, the content of carbon cloth is in 35%-50%.
3. the dissolving of polyborosiloxane according to claim 1-carbon cloth composite plate impregnates hot pressing the preparation method, feature
It is：Carbon cloth be plain weave, twill or satin weave, model 1K, 3K, 6K or 12K of carbon cloth, density 200,
240 or 300g/m3。
4. the dissolving of polyborosiloxane according to claim 1-carbon cloth composite plate impregnates hot pressing the preparation method, feature
It is：Carbon fiber includes two-dimentional carbon cloth and three-dimensional carbon cloth.
5. the dissolving of polyborosiloxane according to claim 1-carbon cloth composite plate impregnates hot pressing the preparation method, feature
It is：The carbon cloth layer structure thickness alternate with polyborosiloxane performed polymer is at least more than 1mm.
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| CN201610605586.3A CN106240126B (en) | 2016-07-29 | 2016-07-29 | Polyborosiloxane-carbon fiber fabric swatch and its dissolving dipping hot pressing the preparation method |
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| CN112920551B (en) * | 2021-03-30 | 2022-02-18 | 吉林大学 | Bionic resin-based carbon fiber composite material and preparation method thereof |
| CN114790121B (en) * | 2022-05-12 | 2023-05-16 | 宁波金鼎紧固件有限公司 | Fastener of heat-resistant high-strength carbon/ceramic material and preparation method thereof |
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