CN1970627A - Cyanate resin/ carbon fiber composite material and its preparing process - Google Patents
Cyanate resin/ carbon fiber composite material and its preparing process Download PDFInfo
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- CN1970627A CN1970627A CN 200610096622 CN200610096622A CN1970627A CN 1970627 A CN1970627 A CN 1970627A CN 200610096622 CN200610096622 CN 200610096622 CN 200610096622 A CN200610096622 A CN 200610096622A CN 1970627 A CN1970627 A CN 1970627A
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Abstract
The invention discloses a making method of cyanate resin/carbon fiber composite material, which comprises the following steps: 1) heating and fusing cyanate resin to form transparent pattern under 80-100 deg.c; insulating 1-3h; adding 1-3% carbon nanometer pipe; insulating under 80-150 deg.c for 2-4h; cooling to indoor temperature; obtaining resin base; 2) adding acetone in the resin base with bulk rate at 1:0.8-1:1.2; allocating glue solution; immersing carbon fiber or carbon fiber cloth in the glue solution; drying; doing hot pressing to mould after the quantity of volatile substance is less than 1%; obtaining the product.
Description
Technical field
The present invention relates to the composition and method of making the same of a kind of thermosetting resin and carbon fiber, relate in particular to a kind of cyanate ester resin/carbon-fibre composite.
Background technology
Cyanate ester resin (Cyanate Ester, CE) be a kind of high-performance thermosetting resin matrix that development in recent years is got up, it has outstanding dielectric properties in wide frequency range, have extremely low water-intake rate, good thermotolerance and comprehensive mechanical property and good processibility simultaneously, these noticeable characteristics make it show great potential aspect polymer matrix composites of preparation structure/function integration.
In order to strengthen the intensity of resin, in resin matrix, add strongthener usually, constitute matrix material, strongthener commonly used is a carbon fiber, can directly add carbon fiber, also can add carbon cloth.The quality of the composite property not only essential property with resin matrix and strongthener is relevant, and also depends on the performance of bonding interface between the two to a great extent.Make cyanate ester resin/carbon-fibre composite be expected to reach based on the intrinsic excellent properties of cyanate ester resin and carbon fiber and comprising the harsh application requiring that sophisticated industry proposed of space flight, aviation, but, there is the low and not good two large problems of flame retardant properties of interlaminar shear strength in the cyanate ester resin/carbon-fibre composite of preparation at present, and this will directly have influence on the use properties and the scope of application of matrix material.
Cause the low reason of interlaminar shear strength to be: because carbon fiber surface is inertia, and the mechanical coupling power between resin matrix is little, thereby cause the interfacial bond property of matrix material relatively poor, the ability to bear of impact weak (especially when suffering low velocity impact), for improving its intensity, roughly can be from resin matrix, fortifying fibre, three aspects, interface are considered, promptly by improving the body intensity of polymkeric substance, interfacial adhesion strength between fiber and the matrix, the structure of rationalization's fibre reinforcement is (as two dimension, 3 D weaving etc.) obtain the matrix material of high interlaminar shear strength.Aforesaid method is all comparatively effective and obtained application, but also has certain problem, can make the bigger potentiality of existing resin system performance as braiding structure, still be method itself no matter from resin system, all help reducing cost, still, this method is difficult to be used in complex construction.In addition, braiding structure causes the bending of fiber inevitably, thereby reduces the mechanical property of matrix material.
Cyanate ester resin itself is inflammable, and modern industry is to have good flame-retarding characteristic to one of material requirement, for addressing this problem, the mode of available technology adopting interpolation fire retardant improves the flame retardant properties of matrix material, yet, the adding fire retardant will reduce the mechanical property of resin, influences the application of matrix material.
So, how to research and develop a kind of preparation method and have important science and construction value with high-performance cyanate ester resin/carbon-fibre composite that suitability is wide, operating procedure simply, also can obtain the interlaminar shear strength height simultaneously, flame retardant resistance is good.
Summary of the invention
The object of the invention provides the preparation method that a kind of while can obtain the cyanate ester resin/carbon-fibre composite of interlaminar shear strength height and good flame-retardance.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of cyanate ester resin/carbon-fibre composite, and its step is as follows:
1) resin heating and melting under 80 ℃～150 ℃ temperature is incubated 1～3h, by weight to transparent, contain 100 parts of cyanate ester resins in the described resin, add 1～3 part of carbon nanotube then, under 80 ℃～150 ℃ temperature, be incubated 2～4h, room temperature to be reduced to obtains resin matrix;
2) volume ratio by 1: 0.8～1: 1.2 adds acetone in above-mentioned resin matrix, is made into glue, and this glue is soaked into carbon fiber or carbon cloth, hang then, after treating that fugitive constituent is by weight＜1%, hot-forming, promptly obtain described cyanate ester resin/carbon-fibre composite.
In the technique scheme, step 2) hot-press molding method in is a prior art, a kind of basic step commonly used is: with step 2) in soaked into resin adhesive liquid and hang after carbon fiber or carbon cloth 80 ℃ down baking 10min finish preheating, be laid in the mould, mould is delivered to 120 ℃～150 ℃ stop 30min down, use the exert pressure of 0.7MPa～1Mpa then, pressurize heats up, solidify 6～9h in 160 ℃～200 ℃, then be cooled to room temperature, cooled sheet material after handling 4h under 230 ℃, promptly obtains cyanate ester resin/carbon-fibre composite again, finishes hot-forming step.
For obtaining better effect, optimized technical scheme is above-mentioned steps 1) described in resin mix under 80～150 ℃ by 100 parts of cyanate ester resins and 1～5 part of Resins, epoxy.
Further technical scheme is, described cyanate ester resin is 4,4 '-two cyanate ester based diphenyl propanes, and described Resins, epoxy is a kind of in bisphenol A type epoxy resin, alicyclic type epoxy resin or the phenol aldehyde type epoxy resin or their combination.
In the technique scheme, described carbon nanotube is Single Walled Carbon Nanotube or multi-walled carbon nano-tubes, or its composition.
Because the technique scheme utilization, the present invention compared with prior art has following advantage:
1. because the present invention has added carbon nanotube in resin matrix, increased its outfield force transmission, thereby improved the body intensity of resin matrix and matrix material, solved interlaminar shear strength problem on the low side in the past in the intensity of thickness direction;
2. common, because the mechanical property of carbon nanotube itself is better, those skilled in the art might reckon with the raising of product strength, and the present application people finds through overtesting, prepared cyanate/carbon-fibre composite has outstanding flame retardant properties after adding carbon nanotube, need not to add fire retardant again, has avoided the influence of fire retardant to the resin mechanical property, thereby obtained beyond thought effect, inferred that its action principle is because carbon nanotube has the effect of heat being played barrier;
3. moulding process of the present invention is simple, suitability is wide, material source is convenient, is beneficial to widely-usedly, is particularly suitable for material mechanical performance, thermal characteristics, the demanding occasion of flame retardant resistance.
Embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment one:
By weight, with 100 part 4,4 '-two cyanate ester based diphenyl propanes are 150 ℃ of fusions, and insulation 3h adds 1 part of multi-walled carbon nano-tubes at 150 ℃ then and mixes with it, behind the insulation 3h, reduces to room temperature and obtains resin matrix, is modified cyanic acid ester resin; In the modified cyanic acid ester resin matrix that makes, add acetone, be mixed with resin adhesive liquid in 1: 1 by volume, above-mentioned glue is brushed on the PX35FBUD0300 carbon cloth, room temperature makes fugitive constituent weight ratio＜1% in the resin matrix after hanging 15h, dry by the fire 10min down at 80 ℃ then and carry out preheating, be laid in the mould, mould sent in thermocompressor suppress.Heat pressing process is: begin pressurization (1MPa) behind 120 ℃ of stop 30min, at 160 ℃, 180 ℃, 200 ℃ each pressurize 2h, then be cooled to room temperature respectively.After compacting finished, the sheet material of taking-up promptly obtained cyanate/carbon-fibre composite at 230 ℃ of aftertreatment 4h.
Do not add carbon nanotube, compare experiment, experimental result is as shown in table 1:
Table 1
| Carbon nanotube | Shearing resistance | Flexural strength | Burning time | The maximum heat release rate | |
| Prior art | Do not have | 65.3MPa | ?722.1MPa | ?75s | ?142kw/m 2 |
| Embodiment 1 | Have | 74.6MPa | ?745.3MPa | ?83s | ?121kw/m 2 |
Contrast table 1 as can be known, under equal conditions, prepared matrix material behind the adding carbon nanotube in the resin matrix, the shearing resistance of interlayer and flexural strength all are higher than and do not add the prepared matrix material of carbon nanotube (being prior art), and burning time is after adding carbon nanotube, the time that is spent is longer, and therefore the maximum heat release rate effectively raises the flame retardant resistance of made matrix material again less than under the state that does not add carbon nanotube after adding carbon nanotube simultaneously.
Embodiment 2
By weight, with 100 part 4,4 '-two cyanate ester based diphenyl propanes and 4 parts of alicyclic type epoxy resin TDE-85 mix down at 100 ℃, the transparent back insulation of thing to be mixed 1h, mix with it at 100 ℃ of adding wall amination carbon nanotubes more than 1 part and 1 part of Single Walled Carbon Nanotube then, behind the insulation 2h, reduce to room temperature and obtain modified resin.In the modified cyanic acid ester resin matrix that makes, add acetone, be mixed with resin adhesive liquid in 1: 1 by volume.Above-mentioned glue is brushed on the PX35FBUD0300 carbon cloth, after at room temperature hanging 15h and drying by the fire 10min 80 ℃ times, is laid in the mould.Mould sent carry out hot pressing in thermocompressor, pressing process is: begin pressurization (1MPa) at 130 ℃ after stopping 30min, at 160 ℃, 180 ℃, 200 ℃ each pressurize 2h, then be cooled to room temperature respectively.After compacting finished, the sheet material of taking-up promptly obtained cyanate/carbon-fibre composite at 230 ℃ of aftertreatment 4h.
Do not add carbon nanotube, compare experiment, experimental result is as shown in table 2:
Table 2
| Carbon nanotube | Shearing resistance | Flexural strength | Burning time | The maximum heat release rate | |
| Prior art | Do not have | 79.9MPa | ?800.8MPa | ?78s | ?148kw/m 2 |
| Embodiment 2 | Have | 94.0MPa | ?860.7MPa | ?85s | ?123kw/m 2 |
Table 2, equal 4, in the mixture resin matrix of 4 '-two cyanate ester based diphenyl propanes and alicyclic type epoxy resin, embodiment 2 adds into carbon nanotube compared to prior art, therefore prepared matrix material is strengthened at interlaminar shear strength and flexural strength; And aspect flame retardant properties, because carbon nanotube has the barrier action to heat, so after adding carbon nanotube in the present embodiment, burning time prolongs, and the maximum heat release rate is reduced simultaneously.
Embodiment 3
By weight, with 100 part 4,4 '-two cyanate ester based diphenyl propanes are 80 ℃ of fusions, and insulation 1h adds 3 parts of single wall amination carbon nanotubes at 80 ℃ then and mixes with it, behind the insulation 4h, reduces to room temperature and obtains the modified cyanic acid ester resin matrix.In above-mentioned resin matrix, add acetone, be mixed with resin adhesive liquid in 1: 1 by volume.Above-mentioned glue is soaked on the IM7 carbon fiber by winding process, after at room temperature hanging 15h and drying by the fire 10min 80 ℃ times, be laid in the mould, mould is sent in thermocompressor, carry out hot pressing.Hot pressing technology is: begin pressurization (1MPa) behind 130 ℃ of stop 30min, at 160 ℃, 180 ℃, 200 ℃ each pressurize 2h, then be cooled to room temperature respectively.After compacting finished, the sheet material of taking-up promptly obtained cyanate/carbon-fibre composite at 230 ℃ of aftertreatment 4h.
Embodiment 4
By weight, 100 part 4,4 '-two cyanate ester based diphenyl propanes and 2 parts of bisphenol A type epoxy resin E51 mix down at 120 ℃, the transparent back insulation of thing to be mixed 2h, add the carbon nanotube of wall acidifying more than 1 part at 100 ℃ then and mix with it, behind the insulation 3h, reduce to room temperature and obtain the modified cyanic acid ester resin matrix, in above-mentioned resin matrix, add acetone, be mixed with resin adhesive liquid in 1: 1 by volume.Above-mentioned glue is brushed on the PX35FBUD0150 carbon cloth, after at room temperature hanging 15h and drying by the fire 10min 80 ℃ times, is laid in the mould.Mould sent carry out hot pressing in thermocompressor, pressing process is: begin pressurization (0.7MPa) at 150 ℃ after stopping 30min, respectively at 180 ℃, 200 ℃ each pressurize 2h, then be cooled to room temperature behind 160 ℃ of pressurize 3h.After compacting finished, the sheet material of taking-up promptly obtained cyanate/carbon-fibre composite at 230 ℃ of aftertreatment 4h.
Embodiment 5
By weight, 100 part 4,4 '-two cyanate ester based diphenyl propanes and 1 part of phenol aldehyde type epoxy resin F44 mix down at 120 ℃, the transparent back insulation of thing to be mixed 2h, add the carbon nanotube of wall acidifying more than 1 part at 100 ℃ then and mix with it, behind the insulation 3h, reduce to room temperature and obtain the modified cyanic acid ester resin matrix, in above-mentioned resin matrix, add acetone, be mixed with resin adhesive liquid in 1: 1 by volume.Above-mentioned glue is brushed on the PX35FBUD0300 carbon cloth, after at room temperature hanging 15h and drying by the fire 10min 80 ℃ times, is laid in the mould.Mould sent carry out hot pressing in thermocompressor, pressing process is: begin pressurization (0.7MPa) at 130 ℃ after stopping 30min, at 160 ℃, 180 ℃, 200 ℃ each pressurize 2h, then be cooled to room temperature respectively.After compacting finished, the sheet material of taking-up promptly obtained cyanate/carbon-fibre composite at 230 ℃ of aftertreatment 4h.
Embodiment 6
By weight, 100 part 4,4 '-two cyanate ester based diphenyl propanes and 3 parts of bisphenol A type epoxy resin E44 and 2 parts of alicyclic type epoxy resin TDE-85 mix down at 100 ℃, the transparent back insulation of thing to be mixed 1h, add the carbon nanotube of wall acidifying more than 1 part at 100 ℃ then and mix with it, behind the insulation 2h, reduce to room temperature and obtain the modified cyanic acid ester resin matrix, in above-mentioned resin matrix, add acetone, be mixed with resin adhesive liquid in 1: 1 by volume.Above-mentioned glue is soaked on the T300 carbon fiber by winding process, after at room temperature hanging 15h and drying by the fire 10min 80 ℃ times, be laid in the mould.Mould sent carry out hot pressing in thermocompressor, pressing process is: begin pressurization (0.7MPa) at 130 ℃ after stopping 30min, at 160 ℃, 180 ℃, 200 ℃ each pressurize 3h, then be cooled to room temperature respectively.After compacting finished, the sheet material of taking-up promptly obtained cyanate/carbon-fibre composite at 230 ℃ of aftertreatment 4h.
Claims (6)
1. the preparation method of a cyanate ester resin/carbon-fibre composite, its step is as follows:
1) resin heating and melting under 80 ℃～150 ℃ temperature is incubated 1～3h, by weight to transparent, contain 100 parts of cyanate ester resins in the described resin, add 1～3 part of carbon nanotube then, under 80 ℃～150 ℃ temperature, be incubated 2～4h, room temperature to be reduced to obtains resin matrix;
2) volume ratio by 1: 0.8～1: 1.2 adds acetone in above-mentioned resin matrix, is made into glue, soaks into carbon fiber or carbon cloth with this glue, hang then, after treating that fugitive constituent is by weight＜1%, hot-forming, promptly obtain described cyanate ester resin/carbon-fibre composite.
2. the preparation method of cyanate ester resin/carbon-fibre composite according to claim 1, it is characterized in that: described resin is mixed under 80～150 ℃ by 100 parts of cyanate ester resins and 1～5 part of Resins, epoxy.
3. the preparation method of cyanate ester resin/carbon-fibre composite according to claim 1 and 2, it is characterized in that: described cyanate ester resin is 4,4 '-two cyanate ester based diphenyl propanes.
4. the preparation method of cyanate ester resin/carbon-fibre composite according to claim 3 is characterized in that: described Resins, epoxy is a kind of in bisphenol A type epoxy resin, alicyclic type epoxy resin or the phenol aldehyde type epoxy resin or their combination.
5. the preparation method of cyanate ester resin/carbon-fibre composite according to claim 1, it is characterized in that: described carbon nanotube is Single Walled Carbon Nanotube or multi-walled carbon nano-tubes, or its composition.
6. adopt the cyanate ester resin/carbon-fibre composite of the method preparation of claim 1.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101665670A (en) * | 2009-09-29 | 2010-03-10 | 中国航空工业集团公司北京航空材料研究院 | Adhesive film material for connecting micro-interface reinforced structural adhesive and preparation method thereof |
| CN101225229B (en) * | 2008-02-04 | 2010-11-10 | 苏州大学 | Wet-heat cyanate ester/ composite material and preparation method thereof |
| CN105199385A (en) * | 2015-09-22 | 2015-12-30 | 苏州博利迈新材料科技有限公司 | Cyanic acid resin for toughness and preparation method thereof |
| CN106009662A (en) * | 2016-07-31 | 2016-10-12 | 长春长光宇航复合材料有限公司 | Controllable-thermal-expansion-coefficient carbon fiber/cyanate composite material and preparation method thereof |
| CN106046782A (en) * | 2016-05-18 | 2016-10-26 | 苏州大学 | Modified cyanate resin and preparation method thereof |
| CN111073499A (en) * | 2019-12-27 | 2020-04-28 | 哈尔滨工业大学 | Preparation method of red flag mark for deep space detector |
| CN114801365A (en) * | 2022-05-27 | 2022-07-29 | 西南科技大学 | High-performance aluminum alloy-carbon fiber reinforced resin matrix composite material and preparation method thereof |
| CN117964996A (en) * | 2024-01-30 | 2024-05-03 | 华中科技大学 | Carbon nanotube resin dispersion-based body lightning-proof carbon fiber composite material and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0266986A3 (en) * | 1986-11-06 | 1989-09-06 | Amoco Corporation | Resin compositions comprising aromatic cyanate esters, polyepoxide compounds and thermplastic polymers and prepreg made therefrom |
| EP0319000B1 (en) * | 1987-12-02 | 1995-03-22 | Canon Kabushiki Kaisha | Ink jet head, substrate therefor, process for preparing thereof and ink jet apparatus having said head |
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2006
- 2006-10-11 CN CNB2006100966224A patent/CN100422261C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101225229B (en) * | 2008-02-04 | 2010-11-10 | 苏州大学 | Wet-heat cyanate ester/ composite material and preparation method thereof |
| CN101665670A (en) * | 2009-09-29 | 2010-03-10 | 中国航空工业集团公司北京航空材料研究院 | Adhesive film material for connecting micro-interface reinforced structural adhesive and preparation method thereof |
| CN101665670B (en) * | 2009-09-29 | 2013-12-25 | 中国航空工业集团公司北京航空材料研究院 | Adhesive film material for connecting micro-interface reinforced structural adhesive and preparation method thereof |
| CN105199385A (en) * | 2015-09-22 | 2015-12-30 | 苏州博利迈新材料科技有限公司 | Cyanic acid resin for toughness and preparation method thereof |
| CN106046782A (en) * | 2016-05-18 | 2016-10-26 | 苏州大学 | Modified cyanate resin and preparation method thereof |
| CN106046782B (en) * | 2016-05-18 | 2018-07-20 | 苏州大学 | A kind of modified cyanic acid ester resin and preparation method thereof |
| CN106009662A (en) * | 2016-07-31 | 2016-10-12 | 长春长光宇航复合材料有限公司 | Controllable-thermal-expansion-coefficient carbon fiber/cyanate composite material and preparation method thereof |
| CN111073499A (en) * | 2019-12-27 | 2020-04-28 | 哈尔滨工业大学 | Preparation method of red flag mark for deep space detector |
| CN114801365A (en) * | 2022-05-27 | 2022-07-29 | 西南科技大学 | High-performance aluminum alloy-carbon fiber reinforced resin matrix composite material and preparation method thereof |
| CN117964996A (en) * | 2024-01-30 | 2024-05-03 | 华中科技大学 | Carbon nanotube resin dispersion-based body lightning-proof carbon fiber composite material and preparation method thereof |
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Assignee: Grand Ease Communication Cable Co., Ltd. Assignor: Soochow University Contract record no.: 2010440001235 Denomination of invention: Cyanate resin/ carbon fiber composite material and its preparing process Granted publication date: 20081001 License type: Exclusive License Open date: 20070530 Record date: 20100818 |
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