KR20170102141A - Semi-prepreg for out-of-autoclave and method for producing the same - Google Patents

Semi-prepreg for out-of-autoclave and method for producing the same Download PDF

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Publication number
KR20170102141A
KR20170102141A KR1020160024707A KR20160024707A KR20170102141A KR 20170102141 A KR20170102141 A KR 20170102141A KR 1020160024707 A KR1020160024707 A KR 1020160024707A KR 20160024707 A KR20160024707 A KR 20160024707A KR 20170102141 A KR20170102141 A KR 20170102141A
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KR
South Korea
Prior art keywords
impregnated
carbon fiber
prepreg
pressing
heating
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KR1020160024707A
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Korean (ko)
Inventor
방윤혁
박상철
김성룡
Original Assignee
주식회사 효성
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Priority to KR1020160024707A priority Critical patent/KR20170102141A/en
Publication of KR20170102141A publication Critical patent/KR20170102141A/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/28—Shaping operations therefor
    • B29C70/30—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/28—Shaping operations therefor
    • B29C70/30—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core
    • B29C70/32—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core on a rotating mould, former or core
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/28—Shaping operations therefor
    • B29C70/30—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core
    • B29C70/34—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core and shaping or impregnating by compression, i.e. combined with compressing after the lay-up operation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs

Abstract

The present invention relates to a process for impregnating a carbon fiber with a resin coated on a release paper,
1) feeding the resin film to the upper and lower surfaces of the carbon fiber sheet;
2) pressing and heating the carbon fiber sheet with the first pressing and heating rollers so that the resin film is impregnated on the lower surface of the laminated carbon film sheet at 10 to 30%;
3) pressing and heating the carbon fiber sheet with the second pressurizing and heating rollers so that the resin film is impregnated with 100% at intervals of 100 mm after the partial impregnation performed in step 2);
4) removing the releasing paper after passing through the second pressurizing and heating rollers, and supplying the releasing film to prepare a prepreg, and to a method of manufacturing the semi-impregnated prepreg for deuteroclave molding.
According to the present invention, there is a feature that a molded article having an excellent workability and a low void content can be obtained by using the semi-impregnated prepreg for de-autoclave molding.

Description

[0001] Semi-prepreg for out-of-autoclave and method for producing the same [0002]

The present invention relates to a semi-impregnated prepreg for de-autoclave molding and a method of manufacturing the same.

When a carbon fiber-reinforced plastic product is manufactured using a conventional prepreg in an intermediate state, a high-pressure and high-temperature curing condition is required, and the autoclave equipment is required at this time. Carbon fiber reinforced plastic products using autoclaves are excellent in quality and performance, but it takes a lot of time for production such as pretreatment for operation of equipment and post-operation time, and the operation cost is high. Thus, the prepreg for the autoclave used in the past has begun to be manufactured for the autoclave for curing in the general oven. In this way, it is possible to: 1) design the resin to be easily discharged at a low pressure by lowering the resin viscosity applied to the prepreg; 2) have a cavity in which the gas can be moved by impregnating the resin only to a predetermined portion of the upper and lower portions of the prepreg The design was applied to the de-autoclave process, or 3) the autoclave-free carbon fiber reinforced plastic product was made by curing the prepreg for general autoclave under de-autoclave conditions.

The registered patent publication No. 10-1528336 (registered on June 5, 2015) discloses a semi-impregnated prepreg for a de-autoclave process which is improved in shape stability and moldability by controlling the viscosity and flowability of the impregnating resin applied on both sides of the fiber A manufacturing method thereof has been introduced, and more particularly, to a method of continuously supplying fibers in a sheet form; A first reinforcing film coated on a release paper with a first thermosetting resin for stabilizing the shape of the fiber is pressed onto one surface of the fiber and has a viscosity lower than that of the first thermosetting resin so as to penetrate the fiber, Pressing a second reinforcing film coated on a release paper with a second thermosetting resin on the other surface of the fiber to form a prepregged fiber; Removing the releasing paper of the first reinforcing film and the releasing paper of the second reinforcing film by passing the prepregized fiber through take-up rolls; And preparing a semi-impregnated prepreg by laminating a protective film on one side of the prepregged fiber from which the releasing paper has been removed and a new releasing paper on the other side to form a semi-impregnated prepreg, Wherein the second thermosetting resin is a high viscosity / low flow resin as compared with the second thermosetting resin so as to maintain the shape stability of the semi-impregnated prepreg, and the second thermosetting resin has a low viscosity / high flowability resin Wherein the first thermosetting resin as the high viscosity / low flow resin has a viscosity of 90,000 to 110,000 cps and a melt flow index of 75 to 85 g / min at 75 to 85 DEG C, and the second thermosetting resin as the second viscosity The thermosetting resin has a viscosity of from 4,000 to 6,000 cps and a melt flow index of from 450 to 800 g / min at 75 to 85 ° C. The first thermosetting resin as the high viscosity / low flow resin and the second thermosetting resin as the low viscosity / 2 thermostat Wherein the ratio of the thickness of the resin to the resin is 1: 2 to 4, and in the step of forming the prepregized fiber, the prepregized fiber is divided into a first heating / pressing roller, a second heating / pressing roller, Pressure roller and the third heating / pressurizing roller, wherein the temperature of the first heating / pressurizing roller is 80 占 폚, the temperature of the second heating / pressurizing roller is 80 占 폚, the temperature of the third heating / Is maintained at a temperature of 25 占 폚. A method of manufacturing a semi-impregnated prepreg for a de-autoclave process is disclosed. Open No. 10-2012-0078455 (published on Jul. 10, 2012) discloses a prepreg manufacturing method in which a resin film is put on upper and lower surfaces of a fiber and then passed between impregnation rollers to impregnate the resin of the resin film on the upper and lower surfaces of the fiber , The temperature of both side portions of the impregnation roller is controlled to be lower than the temperature of the central portion when the resin film and the fiber pass through the impregnation roller. At this time, the temperature of the central portion of the impregnation roller is such that the viscosity of the resin is 10 to 50 cps, and the temperature of both sides is 50 cps or more.

Patent Document 1 of the prior art as described above impregnates only a part of both sides between fiber bundles and Patent Document 2 impregnates the upper and lower surfaces of the fibers and differently applies the viscosity of the upper and lower resin of the prepreg, It is complicated and has a drawback that a peeling phenomenon or a gap is generated in the prepreg lamination.

Accordingly, it is an object of the present invention to provide a semi-impregnated prepreg for deoautoclave molding, which can simplify the process and reduce the peeling phenomenon in the non-impregnated section that can occur in the prepreg lamination process, and a method of manufacturing the same. .

In order to achieve the above object, the present invention provides a process for impregnating a carbon fiber with a resin film coated on a release paper by a semi-impregnated prepreg for de-autoclave molding and a method for producing the same, To the resin film; 2) pressing and heating the carbon fiber sheet with the first pressing and heating rollers so that the resin film is impregnated on the lower surface of the laminated carbon film sheet at 10 to 30%; 3) pressing and heating the carbon fiber sheet with the second pressurizing and heating rollers so that the resin film is impregnated into the carbon fiber sheet after the partial impregnation in step 2) at 100 to 150 mm intervals; 4) removing the release paper after passing through the second pressurizing and heating roller, and supplying the releasing film, and a method of manufacturing the semi-impregnated prepreg for deacetoclave molding.

Wherein the resin film is impregnated on at least one surface of the carded carbon fiber sheet in an amount of 10 to 30% of the total area, and is impregnated with 100% in 100 mm intervals. to provide.

The semi-impregnated prepreg for de-autoclave molding of the present invention and its manufacturing method do not use the autoclave which occupies the largest equipment and operation cost in manufacturing carbon fiber-reinforced plastic, The present invention is advantageous in that it can be manufactured by simply changing the manufacture setting of a commonly used equipment. In addition, since the same resin is used, the manufacturing process is simple, and the 100% impregnated spot spaced apart at regular intervals has an effect of reducing defects (peeling phenomenon or fiber cracking) occurring in the curved surface lamination or in the non-impregnated section during pressing.

1 is a process diagram of a method for producing a semi-impregnated prepreg for de-autoclave molding according to the present invention.
2 is a vertical cross-sectional view of a semi-impregnated prepreg for de-autoclave molding according to the present invention.
3 is a plan view of Fig.

Hereinafter, the present invention will be described in detail with reference to the accompanying drawings. However, the following description is intended to illustrate the present invention, and the present invention is not limited thereto.

FIG. 1 is a process drawing showing a method of manufacturing a semi-impregnated prepreg for deacetyl forming according to the present invention.

1, the resin films 122a and 122b coated on the coated paper are first fed to the upper and lower surfaces of the carbon fiber sheet 110 (step 1) step). The resin used for the resin films 122a and 122b may be a thermosetting resin selected from the group consisting of epoxy, phenol, polyester, bismaleide, and mixtures thereof, or a mixture of nylon, polypropylene, polycarbonate, , And an epoxy resin is used in the embodiment of the present invention.

Next, the carbon fiber sheet 110 having the resin films 122a and 122b laminated thereon is pressed and heated by the first pressing and heating rollers 130a and 130b so that the resin films 122a and 122b are impregnated ). The first pressing and heating rollers 130a and 130b are composed of two rollers facing each other. The first pressing and heating rollers 130a and 130b are pressed and heated at a pressure of 5 to 20 N at 120 to 180 ° C for 1 second, It is preferable that the resin films 122a and 122b are impregnated on the upper and lower surfaces at 10 to 30%. If the temperature of the first pressurization and heating rollers 130a and 130b is below 120 ° C, the resin can not be impregnated into the carbon fibers. If the temperature is above 180 ° C, the fluidity of the resin increases and penetrates deeply into the interior of the prepreg. If the pressure is less than 5 N, the pressing force is weak and the impregnation is disadvantageous. If the pressure is more than 20 N, the impregnated region becomes deep. If the carbon fiber sheet 110 is impregnated with less than 10% of the resin film 122a or 122b, the workability of the prepreg deteriorates. If the carbon fiber sheet 110 is impregnated by 30% or more, the air fluidized bed becomes narrower, give. In the embodiment of the present invention, the resin films 122a and 122b are impregnated with 20% by pressurization and heating at 150 DEG C and 10 N, for example.

After the second step, the carbon fiber sheet 110 is pressed and heated by the second pressurizing and heating rollers 140a and 140b so that the resin films 122b and 122b are impregnated with 100% at intervals of 50 to 150 mm ). The second pressing and heating rollers 140a and 140b are composed of two rollers facing each other and the second pressing and heating rollers 140a and 140b are formed on the surfaces of the second pressing and heating rollers 140a and 140b. And a plurality of protrusions 142 are formed at intervals of 50 to 150 mm in the circumferential direction. If the distance between the plurality of protrusions 142 is 50 mm or less, overlapping occurs in the 100% impregnated region, and airflow is difficult to be generated. If the spacing is 150 mm or more, workability such as fiber cracking is reduced. The second pressurizing and heating rollers 140a and 140b having the plurality of protrusions 142 are pressurized and heated at a pressure of 40 to 60 N at 120 to 180 ° C for 1 second to form 50 It is preferable that the resin films 122a and 122b are impregnated with 100% at intervals of 150 mm. If the temperature of the second pressurization and heating rollers 140a and 140b is below 120 ° C, 100% impregnation is difficult to reach the inside of the prepreg, and if it is 150 ° C or higher, resin induction increases and partial impregnation becomes difficult. If the pressure is below 40 N, 100% impregnation is difficult. If the pressure is above 60 N, the fiber will be damaged by excessive pressure. In the embodiment of the present invention, the resin films 122a and 122b are impregnated with 100% at intervals of 100 mm on the carbon fiber sheet 110 by pressurization and heating, for example, at 150 ° C and 50 N.

Finally, the coated paper 152a, 152b used for resin impregnation is removed from the take-up rolls 150a, 150b after passing through the second pressurizing and heating rollers 140a, 140b, and is discharged to the second feeders 160a, The film 162a and release paper 162b are fed to produce a semi-impregnated prepreg 170 (step 4).

The coated paper 152a and 152b are heated by the first pressing and heating roller 130a and 130b and the melted resin film and the first pressing and heating roller during the second pressing and heating rollers 140a and 140b, And the coated paper 152a, 152b are recovered through the take-up rolls 150a, 150b after the first pressurization and heating roller and the second pressurization and heating roller process. In addition, when the coated paper 152a and 152b are recovered, the release film 162a and the release paper 162b are laminated on the second supply devices 160a and 160b to prevent them from sticking to each other when the semi-impregnated prepreg 170 is wound, Impregnated prepreg 170 according to the present invention.

FIG. 2 is a vertical cross-sectional view of the prepreg showing the structure of the thus fabricated semi-impregnated prepreg for autoclave molding. 2, the carbon fiber sheet was impregnated with 10 to 30% of the upper and lower surfaces, and the carbon fiber sheet was impregnated with 100% A prepreg can be produced.

The semi-impregnated prepreg for autoclave molding was impregnated with 10 to 30% of the upper and lower surfaces of the carbon fiber sheet and 100% of the carbon fiber sheets were impregnated at intervals of 100 mm. Thus, It is effective to reduce the peeling phenomenon and the fiber cracking phenomenon occurring in the non-impregnated zone.

That is, in the manufacturing process of the carbon fiber-reinforced plastic in which the vacuum impregnated pre-impregnation pretreatment for de-autoclave molding is carried out, 1) a flow path through which air can move through the unimproved region of the intermediate portion of the prepreg is made, 2) It is possible to provide a prepreg capable of producing a carbon fiber-reinforced plastic product of higher quality without autoclave by removing air (voids) in the product molding space by a vacuum blanking operation in the oven.

Hereinafter, the present invention will be described in more detail with reference to the following embodiments. It is to be understood that the same is by way of illustration and example only and is not to be taken by way of limitation.

[Example]

Carbon fiber (Hyosung H2550 12K) is opened in a 30 cm width facility, and the carbonized fiber is passed between the resin-coated films to make a carbon fiber sheet having a fiber weight of 190 g / mm 2 per unit area. The coating film used was applied on the release film so that the resin was 50 g / mm 2 . The carded carbon fiber, which is piled up with the coating film on the top and bottom, is passed between the first pressurizing and heating rollers at a high temperature of 150 ° C and compressed at a pressure of 10 N for 1 second to impregnate 20% of the lower surface of the carbon fiber sheet.

After passing through a second pressurizing and heating roller at a high temperature of 150 占 폚 capable of partial impregnation, the resin is pressed at 50 N for 1 second to impregnate 100% of the resin with carbon fibers at intervals of 100 mm. The diameters of the first pressurizing and heating rollers and the second pressurizing and heating rollers used were 300 mm. After releasing the release paper after passing through the second pressurizing and heating roller, a releasing film was applied to produce an article prepreg.

[ Comparative Example ]

Comparative Example  One

Referring to FIG. 1, the pressure applied to the second pressurizing and heating roller was lowered to 10 N to prepare a prepreg, and the rest of the process was applied in the same manner as the embodiment.

Comparative Example  2

Referring to FIG. 1, the shape of the second pressurizing and heating roller is replaced with a projection-free shape such as the first pressurizing and heating roller so that a 20% partial impregnation region can be impregnated up to 60-80% The second pressurizing and heating rollers are squeezed at a pressure of 50 N for 1 second to partially impregnate at a higher rate than in the Examples. The remaining steps were applied in the same manner as in the examples.

[ Experimental Example ]

A carbon fiber composite material structure having a curved shape was prepared by performing a de-autoclave process on a semi-impregnated prepreg prepared by the method of Example, Comparative Example 1, and Comparative Example 2. The comparison items were evaluated for processability (cuttability, workability, handling), lamination process (lamination property, workability), and final molding quality (porosity).

As shown in Table 1, the prepreg was cut to prepare the process, and the workability of handling the laminate for removing the release film was the best in Comparative Example 2. It can be seen that many 60 to 80% of the resin is impregnated into the carbon fiber to make the internal state solid, while the relatively small 20% partially impregnated prepreg also shows excellent process readiness due to the 100% spot impregnated region there was.

For reasons similar to workability, prepregs that are solid inside (when the amount of resin impregnated is large) showed stable workability in the lamination process. However, in the case of Comparative Example 2, it was confirmed that there was a small amount of the non-impregnation zone secured by the air passage, which was difficult in defoaming the internal air after the lamination operation. Since the vacuum autoclave process uses a vacuum bag alone, it is confirmed that the embodiment and the comparative example 1 have excellent workability.

In addition, it was confirmed that the structure was laminated in the 'a' form, and the interlaminar peeling (slip) occurring in the non-impregnated region and the fiber cracking in the curved surface were confirmed, and the 100% spot impregnated region of the example improved the lamination workability.

The most important process evaluation items in the present invention are that the autoclave work requires a short vacuum time and a low void content in the molded article under these conditions, It appeared best.

Representative evaluation items Detailed evaluation items Example Comparative Example 1 Comparative Example 2 Preparation process Cutting Fiber crevices at cutting ○ X ◎ Workability Interlayer stability when removing release film ◎ X ◎ Handleability Prepreg shape stability (handling) ○ △ ◎ Lamination process Lamination property Tack (Bonding between prepregs) ○ ○ △ Workability Non-impregnated area during lamination Slip Yes / No ◎ X ◎ Fiber cracking during curved surface lamination ◎ △ ◎ Vacuum working time ○ ◎ X Molding quality Porosity Particle voids content ◎ ○ X

⊚: very good (no) ∘: good △: fair X: poor (poor)

100: Semi-impregnated prepreg step 110: Carbon fiber sheet
120a, 120b: first feeding device 122a, 122b: resin film
130a, 130b: first pressing and heating roller 140a, 140b: second pressing and heating roller
142: projections 150a and 150b: take-up roll
152a, b: Coated paper 160a, 160b: Second feeding device
162a: release film 162b: release paper
170: Semi-impregnated prepreg

Claims (6)

In the step of impregnating the carbon fiber with the resin film coated on the release paper,
1) feeding the resin film to the upper and lower surfaces of the carbon fiber sheet;
2) pressing and heating the carbon fiber sheet with the first pressing and heating rollers so that the resin film is impregnated on the lower surface of the laminated carbon film sheet at 10 to 30%;
3) pressing and heating the carbon fiber sheet with the second pressurizing and heating rollers so that the resin film is impregnated into the carbon fiber sheet after the partial impregnation in step 2) at 100 to 150 mm intervals;
4) removing the release paper after passing through the second pressurizing and heating roller, and supplying the releasing film. The method of claim 1, wherein the first pressing and heating rollers are pressurized and heated at a pressure of 5 to 20 N at a temperature of 120 to 180 ° C so that the resin film is impregnated on the lower surface of the carbon fiber sheet at 10 to 30% Impregnated prepreg for forming autoclave. The method as claimed in claim 1, wherein the second pressurizing and heating roller is pressurized and heated at a pressure of 40 to 60 N at a temperature of 120 to 180 DEG C to impregnate the carbon fiber sheet with the resin film at 100 to 100% By weight based on the total weight of the semi-impregnated prepreg. The method of claim 1 or 3, wherein a surface of the second pressing and heating roller is protruded along the longitudinal direction of the second pressing and heating roller, and a plurality of protrusions are spaced apart from each other by 50 to 150 mm in the circumferential direction By weight based on the total weight of the semi-impregnated prepreg. The method of claim 1, wherein the resin film is selected from the group consisting of thermosetting resins selected from the group consisting of epoxy, phenol, polyester, bismaleide, and mixtures thereof, or nylon, polypropylene, polycarbonate, Impregnated prepreg for de-autoclave molding, wherein the thermoplastic resin is a thermoplastic resin. Characterized in that the resin film according to any one of claims 1 to 5 is impregnated on at least one surface of the carded carbon fiber sheet in an amount of 10 to 30% Impregnated impregnated prepreg.
KR1020160024707A 2016-02-29 2016-02-29 Semi-prepreg for out-of-autoclave and method for producing the same KR20170102141A (en)

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