CN109895416B - Forming method of phthalonitrile composite material thin-wall curved surface shell - Google Patents

Forming method of phthalonitrile composite material thin-wall curved surface shell Download PDF

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CN109895416B
CN109895416B CN201910228097.4A CN201910228097A CN109895416B CN 109895416 B CN109895416 B CN 109895416B CN 201910228097 A CN201910228097 A CN 201910228097A CN 109895416 B CN109895416 B CN 109895416B
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phthalonitrile
temperature
composite material
correction treatment
deformation
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CN109895416A (en
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史汉桥
孙宝岗
雷琴
杨昆晓
王俊山
孙宏杰
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China Academy of Launch Vehicle Technology CALT
Aerospace Research Institute of Materials and Processing Technology
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China Academy of Launch Vehicle Technology CALT
Aerospace Research Institute of Materials and Processing Technology
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Abstract

The invention relates to a method for forming a phthalonitrile composite thin-wall curved shell, in particular to a method for forming a phthalonitrile composite thin-wall curved shell with low porosity and few defects, which can be applied to the forming of high-temperature-resistant supporting members, high-temperature-resistant protective covers, high-temperature-resistant connecting members and the like, wherein the thin wall is not more than 2mm in wall thickness. The product prepared by the phthalonitrile composite material curved surface shell molding technology has high temperature resistance level, few defects and high profile precision, and can be applied to molding of high-temperature-resistant supporting members, high-temperature-resistant protective covers, high-temperature-resistant connecting members and the like.

Description

Forming method of phthalonitrile composite material thin-wall curved surface shell
Technical Field
The invention relates to a method for forming a phthalonitrile composite thin-wall curved shell, in particular to a method for forming a phthalonitrile composite thin-wall curved shell with low porosity and few defects, which can be applied to the forming of high-temperature-resistant supporting members, high-temperature-resistant protective covers, high-temperature-resistant connecting members and the like, wherein the thin wall is not more than 2mm in wall thickness.
Background
In the field of high-temperature-resistant resin-based structural composite materials, because small molecules are released in the curing process of a traditional high-temperature-resistant resin system, the prepared high-temperature-resistant composite material is high in porosity and usually larger than 1%. The traditional high-temperature resistant resin has the problems of high porosity and poor manufacturability, and is easy to cause large-area loosening, large-area air holes or layering of a high-temperature resistant composite material, so that the quality of a high-temperature resistant composite material product is uncontrollable, and the engineering application of the high-temperature resistant resin matrix structure composite material is seriously restricted.
The curing temperature of the high-temperature-resistant composite material is high, and after the composite material is cured and cooled to room temperature, due to the existence of curing stress and thermal stress inside the composite material and the anisotropic characteristics of the composite material, the product is easy to deform and warp, the size precision of the product is influenced, the size of the product is easy to be out of tolerance, and the application effect of the product is finally influenced. For the structural form of the thin-wall curved shell, the problem of warping deformation of the high-temperature-resistant composite material is more prominent, and the popularization and application of the high-temperature-resistant resin-based structural composite material are severely restricted.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method for molding the thin-wall curved shell made of the phthalonitrile composite material overcomes the defects in the prior art, and the product prepared by the phthalonitrile composite material curved shell molding technology is high in temperature resistance level, few in defects and high in molded surface precision.
The technical solution of the invention is as follows:
a method for forming a phthalonitrile composite material thin-wall curved surface shell comprises the following steps:
(1) carrying out phthalonitrile prepreg laying on a mould, and vacuumizing and compacting;
(2) after the double-layer vacuum bag is adopted for coating, heating is carried out for pretreatment, and silicon rubber is adopted for auxiliary pressurization in the pretreatment process;
(3) after the pretreatment is finished, heating for curing, cooling to room temperature after the curing is finished, and removing the auxiliary coating material to obtain a phthalonitrile cured product;
(4) and (4) applying pressure to the phthalonitrile condensate obtained in the step (3) to perform deformation correction treatment, so as to obtain the phthalonitrile composite material thin-wall curved shell.
In the step (1), the vacuum degree of vacuumizing compaction is less than or equal to-0.095 MPa, and the compaction time of vacuumizing compaction is 20-35 min.
In the step (2), the heating temperature is 150-.
In the step (3), the curing temperature is 240-260 ℃, and the curing time is 3-8 h.
In the step (4), the deformation correction treatment temperature is 300-400 ℃, the deformation correction treatment amount is 2-4 times of the deformation amount, the deformation correction treatment direction is opposite to the deformation direction of the phthalonitrile condensate, and the deformation correction treatment time is 3-6 h.
Compared with the prior art, the method for forming the phthalonitrile composite material thin-wall curved surface shell with controllable quality has the following advantages:
(1) the area occupied by the flaw detection defects of the product prepared by the method is less than 5 percent;
(2) the distance tolerance between the farthest points on the curved surface of the product prepared by the method of the invention is reduced to below 1/10 of the method of the prior art;
(3) a method for forming a phthalonitrile composite material thin-wall curved surface shell with controllable quality comprises the steps of (1) carrying out phthalonitrile prepreg laying on a mould, and vacuumizing and compacting; (2) after being coated by a double-layer vacuum bag, the mixture is heated to 150 to 180 ℃ for pretreatment for 1 to 1.5 hours, and silicon rubber is adopted for auxiliary pressurization;
(3) heating to 240-260 ℃ for curing for 3-8h, and removing the auxiliary coating material after cooling; (4) according to the deformation condition of the product, carrying out deformation correction by a reverse quantitative distance control method, wherein the reverse control distance is 2-4 times of the deformation amount, and the deformation correction treatment temperature is 300-400 ℃.
(4) The product prepared by the phthalonitrile composite material curved surface shell molding technology has high temperature resistance level, few defects and high profile precision, and can be applied to molding of high-temperature-resistant supporting members, high-temperature-resistant protective covers, high-temperature-resistant connecting members and the like.
Drawings
FIG. 1 is a schematic flow chart of the method of the present invention.
Detailed Description
A method for forming a phthalonitrile composite material thin-wall curved surface shell comprises the following steps:
(1) performing phthalonitrile prepreg laying on a mould, vacuumizing and compacting, wherein the vacuum degree is less than or equal to-0.095 MPa, and the compacting time is 20-35 min;
(2) after being coated by a double-layer vacuum bag, the coating is heated to 150-;
(3) heating to 240 ℃ and 260 ℃ for curing for 3-8h, and removing the auxiliary coating material after cooling; auxiliary coating, namely a double-layer vacuum bag and a mould, to obtain a phthalonitrile condensate;
(4) and (3) applying pressure to the phthalonitrile condensate obtained in the step (3) to perform deformation correction treatment, wherein the deformation correction treatment temperature is 300-400 ℃, the deformation correction treatment amount is 2-4 times of the deformation amount, the deformation correction treatment direction is opposite to the deformation direction of the phthalonitrile condensate, and the deformation correction treatment time is 3-6h, so that the phthalonitrile composite thin-wall curved shell is obtained.
The present invention is described in further detail below by way of specific examples.
Example 1
The method for molding the curved shell made of the phthalonitrile composite material comprises the following steps:
(1) carrying out phthalonitrile prepreg laying on a mould, vacuumizing and compacting, wherein the vacuum degree is-0.098 MPa, and the compacting time is 25 min;
(2) after being coated by a double-layer vacuum bag, the mixture is heated to 150 ℃ for pretreatment for 1.5h, and simultaneously, silicon rubber is used for auxiliary pressurization, wherein the thickness of the silicon rubber is 2 mm;
(3) heating to 240 ℃ for curing for 8h, cooling, and removing the double-layer vacuum bag and the mould to obtain a phthalonitrile composite material cured substance;
(4) and (3) applying pressure to the cured phthalonitrile composite material obtained in the step (3) to perform deformation correction treatment, wherein the deformation correction treatment temperature is 400 ℃, the deformation correction treatment amount is 2 times of the deformation amount, the deformation correction treatment direction is opposite to the deformation direction of the cured phthalonitrile material, and the deformation correction treatment time is 6 hours, so that the thin-wall curved shell of the phthalonitrile composite material is obtained.
Flaw detection is carried out on the obtained phthalonitrile composite material thin-wall curved surface shell, and the flaw detection result is that the area occupied by flaw detection defects is 4%; the tolerance of the distance between the furthest two points on the product's curved surface is reduced to 1/12 of the prior art.
Example 2
The method for molding the curved shell made of the phthalonitrile composite material comprises the following steps:
(1) performing phthalonitrile prepreg laying on a mould, vacuumizing and compacting, wherein the vacuum degree is-0.099 MPa, and the compacting time is 20 min;
(2) after being coated by a double-layer vacuum bag, the coating is heated to 180 ℃ for pretreatment for 1h, and simultaneously, silicon rubber is used for auxiliary pressurization, wherein the thickness of the silicon rubber is 3 mm;
(3) heating to 260 ℃ for curing for 3h, cooling, and removing the double-layer vacuum bag and the mould to obtain a phthalonitrile composite material cured substance;
(4) and (3) applying pressure to the cured phthalonitrile composite material obtained in the step (3) to perform deformation correction treatment, wherein the deformation correction treatment temperature is 300 ℃, the deformation correction treatment amount is 4 times of the deformation amount, the deformation correction treatment direction is opposite to the deformation direction of the cured phthalonitrile material, and the deformation correction treatment time is 3 hours, so that the thin-wall curved shell of the phthalonitrile composite material is obtained.
Flaw detection is carried out on the obtained phthalonitrile composite material thin-wall curved surface shell, and the flaw detection result is that the area occupied by flaw detection defects is 2%; the tolerance of the distance between the furthest two points on the product's curved surface is reduced to 1/15 of the prior art.
Example 3
The method for molding the curved shell made of the phthalonitrile composite material comprises the following steps:
(1) carrying out phthalonitrile prepreg laying on a mould, vacuumizing and compacting, wherein the vacuum degree is-0.097 MPa, and the compacting time is 35 min;
(2) after being coated by a double-layer vacuum bag, the coating is heated to 170 ℃ for pretreatment for 1.2h, and simultaneously, silicon rubber is used for auxiliary pressurization, wherein the thickness of the silicon rubber is 1 mm;
(3) heating to 250 ℃ for curing for 5h, cooling, and removing the double-layer vacuum bag and the mould to obtain a phthalonitrile composite material cured substance;
(4) and (3) applying pressure to the cured phthalonitrile composite material obtained in the step (3) to perform deformation correction treatment, wherein the deformation correction treatment temperature is 350 ℃, the deformation correction treatment amount is 3 times of the deformation amount, the deformation correction treatment direction is opposite to the deformation direction of the cured phthalonitrile material, and the deformation correction treatment time is 5 hours, so that the thin-wall curved shell of the phthalonitrile composite material is obtained.
Flaw detection is carried out on the obtained phthalonitrile composite material thin-wall curved surface shell, and the flaw detection result is that the area occupied by flaw detection defects is 3%; the tolerance of the distance between the furthest two points on the product's curved surface is reduced to 1/11 of the prior art.
Example 4
The method for forming the o-phthalonitrile composite material curved surface shell with controllable quality comprises the following steps:
(1) performing phthalonitrile prepreg laying on a mould, vacuumizing and compacting, wherein the vacuum degree is-0.099 MPa, and the compacting time is 20 min;
(2) after being coated by a double-layer vacuum bag, the coating is heated to 160 ℃ for pretreatment for 1.4h, and simultaneously, silicon rubber is used for auxiliary pressurization, wherein the thickness of the silicon rubber is 3 mm;
(3) heating to 255 ℃ for curing for 7h, cooling, and removing the double-layer vacuum bag and the mould to obtain a phthalonitrile composite material cured substance;
(4) and (3) applying pressure to the cured phthalonitrile composite material obtained in the step (3) to perform deformation correction treatment, wherein the deformation correction treatment temperature is 360 ℃, the deformation correction treatment amount is 3.5 times of the deformation amount, the deformation correction treatment direction is opposite to the deformation direction of the cured phthalonitrile material, and the deformation correction treatment time is 4 hours, so that the thin-wall curved shell of the phthalonitrile composite material is obtained.
Flaw detection is carried out on the obtained phthalonitrile composite material thin-wall curved surface shell, and the flaw detection result is that the area occupied by flaw detection defects is 1%; the tolerance of the distance between the furthest two points on the product's curved surface is reduced to 1/13 of the prior art.
Those skilled in the art will appreciate that those matters not described in detail in the present specification are well known in the art.

Claims (1)

1. A method for forming a phthalonitrile composite material thin-wall curved surface shell is characterized by comprising the following steps:
(1) carrying out phthalonitrile prepreg laying on a mould, and vacuumizing and compacting;
(2) after the double-layer vacuum bag is adopted for coating, heating is carried out for pretreatment, and silicon rubber is adopted for auxiliary pressurization in the pretreatment process;
(3) after the pretreatment is finished, heating for curing, cooling to room temperature after the curing is finished, and removing the auxiliary coating material to obtain a phthalonitrile cured product;
(4) applying pressure to the phthalonitrile condensate obtained in the step (3) to perform deformation correction treatment to obtain a phthalonitrile composite material thin-wall curved shell;
in the step (1), the vacuum degree of vacuumizing compaction is less than or equal to-0.095 MPa;
in the step (1), the compaction time of vacuumizing and compacting is 20-35 min;
in the step (2), the heating temperature is 150-180 ℃;
in the step (2), the pretreatment time is 1-1.5 h;
in the step (2), the thickness of the silicon rubber is 1-3 mm;
in the step (3), the curing temperature is 240-260 ℃;
in the step (3), the curing time is 3-8 h;
in the step (4), the deformation correction treatment temperature is 300-400 ℃, and the deformation correction treatment amount is 2-4 times of the deformation amount;
in the step (4), the deformation correction treatment direction is opposite to the deformation direction of the phthalonitrile condensate, and the deformation correction treatment time is 3-6 h.
CN201910228097.4A 2019-03-25 2019-03-25 Forming method of phthalonitrile composite material thin-wall curved surface shell Active CN109895416B (en)

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Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7186367B2 (en) * 2004-05-13 2007-03-06 The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration Double vacuum bag process for resin matrix composite manufacturing
US8628639B2 (en) * 2011-05-28 2014-01-14 The Boeing Company Vacuum bag processing using dual seals
CN102555232A (en) * 2012-01-10 2012-07-11 江苏澳盛复合材料科技有限公司 Process and device for multilayer bag pressing production of fibrous composite plates
CN106391771A (en) * 2016-11-11 2017-02-15 重庆动沃机车产业有限公司 Machine part correction method
CN107031069B (en) * 2017-04-21 2019-07-30 中国电子科技集团公司第五十四研究所 A kind of hard and soft composable mold and its manufacturing method of airborne blade antenna cover
CN108454135B (en) * 2018-01-31 2020-07-14 航天材料及工艺研究所 Phthalonitrile resin prepreg, composite material and preparation method thereof

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