CN110001092A - A kind of phenolic resin preimpregnation material and metalwork integral formation method - Google Patents
A kind of phenolic resin preimpregnation material and metalwork integral formation method Download PDFInfo
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- CN110001092A CN110001092A CN201910408641.3A CN201910408641A CN110001092A CN 110001092 A CN110001092 A CN 110001092A CN 201910408641 A CN201910408641 A CN 201910408641A CN 110001092 A CN110001092 A CN 110001092A
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- phenolic resin
- type face
- transition zone
- metalwork
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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
- B29C70/68—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts by incorporating or moulding on preformed parts, e.g. inserts or layers, e.g. foam blocks
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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
- B29C70/68—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts by incorporating or moulding on preformed parts, e.g. inserts or layers, e.g. foam blocks
- B29C70/681—Component parts, details or accessories; Auxiliary operations
- B29C70/683—Pretreatment of the preformed part, e.g. insert
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Composite Materials (AREA)
- Mechanical Engineering (AREA)
- Lining Or Joining Of Plastics Or The Like (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention relates to a kind of phenolic resin preimpregnation material and metalwork integral formation method.Include: the pretreated step of (1) metalwork: blast processing being carried out to the type face that metalwork needs to be bonded, then the brushwork gelatin on metal mold face；(2) the compound transition zone on through step (1) treated type face the step of；(3) the step of material carries out laying: the brushing phenolic resin adhesive on the type face for be compounded with transition zone is presoaked to phenolic resin, then by phenolic resin preimpregnation material according to designed ply stacking-sequence and thickness laying；The phenolic resin adhesive includes 100 parts by weight of phenolic resin, nbr carboxyl terminal 100-120 parts by weight, dispersing agent 0.5-1 parts by weight；(4) the step of solidifying.This method overcomes the shortcomings of existing forming technique, provide it is a kind of can guarantee the integrally formed of complex profile structural member, solve the problems, such as interfacial detachment after composite material and metal cabin are integrally formed.
Description
Technical field
The present invention relates to molding component technical fields more particularly to a kind of phenolic resin preimpregnation material to be integrally formed with metalwork
Method.
Background technique
With the development of aeronautical and space technology, space has become " commanding elevation " safeguarded national security with interests, Ge Geguo
More and more sight are all invested the development of aircraft by family.Anti- heat problem is to determine the safety of aircraft and smoothly complete items
One of most critical factor of task, and simple with its, the reliable always feature of ablative thermal protection enjoys great popularity, therefore it is all the time
It is all the focus of various countries space flight mechanism and Experts ' Attention.
At this stage, as various technical requirements are higher and higher, product type face becomes increasingly complex, and Wall-Thickness Difference is increasing.It presses
Traditional mould pressing method, molding complex profile outside protect when need to there are more surpluses, then add by machine respectively obtain it is outer prevent
Sheath, it is finally Nian Jie with metal cabin again.Not only process is long for the outer Protection Product of production components in this way, and processing is complicated cumbersome and zero
After component-level bonding, product surface can have splicing gap, and there are risks when use.Therefore, the integrally formed complexity of integration
Moulding surface structure part has become the trend of product design, and the globality of product not only can be improved in the integrally formed structural member of integration
And reliability, and production process is simplified, improve production efficiency.
Because of the essence of phenolic aldehyde strand crosslinking curing, lead to its high problem of condensation curing shrinking percentage, so composite material
Be integrally formed in cabin often because linear expansion coefficient mismatch caused by with metal interface unsticking the problems such as.It is de- to solve in engineering
Viscous problem, people often solve problems as straining isolated layer using 9621 film for rubber or other epoxies adhesive, but
Because the new material introduced will cause the increase of bonding interface, aircraft (cabin) specific moulding is added, inevitably will cause
Stress raisers region, therefore still will appear local unsticking phenomenon.
Summary of the invention
The invention solves technology solve the problems, such as be: overcome the shortcomings of existing forming technique, provide one kind can guarantee it is multiple
Miscellaneous moulding surface structure part it is integrally formed, solve the problems, such as interfacial detachment after composite material and metal cabin are integrally formed.
In order to solve the above-mentioned technical problems, the present invention provides following technical solutions:
A kind of phenolic resin preimpregnation material and metalwork integral formation method, comprising:
(1) the pretreated step of metalwork: blast processing is carried out to the type face that metalwork needs to be bonded, then in metal mold
Brushwork gelatin on face；
(2) the compound transition zone on through step (1) treated type face the step of；
(3) the step of material carries out laying: the brushing phenolic resin on the type face for be compounded with transition zone is presoaked to phenolic resin
Adhesive, then by phenolic resin preimpregnation material according to designed ply stacking-sequence and thickness laying；The phenolic resin adhesive
Include 100 parts by weight of phenolic resin, nbr carboxyl terminal 100-120 parts by weight, dispersing agent 0.5-1 parts by weight；
(4) the step of solidifying.
Preferably, solidified using solidification of hot-press tank method.
Preferably, the solidification of hot-press tank method carries out as follows:
It is warming up to 90-100 DEG C, pressurize 0.5MPa, keeps the temperature 1-1.5h；
It is warming up to 115-125 DEG C, pressurize 0.8MPa, keeps the temperature 2-2.5h；
It is warming up to 155-165 DEG C, keeps the temperature 4-4.5h；
Stop heating, it is with pressure be cooled to 60 DEG C hereinafter, rate of pressure reduction less than 2 DEG C/min.
Preferably, the step (2) includes: the step of preparing transition zone；The step of adhesive transition layer；With the step of vulcanization
Suddenly.
Preferably, the transition zone is 9621 nitrile rubber transition zones.
Preferably, vulcanized at 90-95 DEG C, vulcanization time is preferably 2-2.5h.
Preferably, described the step of preparing transition zone includes: the type face region for dividing metallic object, cuts out 9621 nitrile rubbers
Size, with acetone by 9621 nitrile rubber wiped cleans.
Preferably, the step of adhesive transition layer includes: and applies on the type face of 9621 nitrile rubbers and metallic object respectively
Then brush coating liquid is successively bonded on metallic object according to the region of segmentation.
Preferably, the dispersing agent is selected from polyvinyl alcohol and/or polypyrrole alkanone.
Preferably, after solidification further include mach step: three-dimensional digital-to-analogue is carried out to the product outer profile after solidification
Processing.
Beneficial effect
Above-mentioned technical proposal of the invention has the advantages that
Metal blast " can beat surface rough " before being bonded, and improve bonding quality.Theoretically after metalwork blast in three days
It can use.Glue a thin layer of in external coating in time, can influence rubber because being oxidized to avoid blast region after blast processing
Film bonding quality.
It is traditional using 9621 film for rubber or other epoxies adhesive as straining isolated layer when, only select a kind of gluing
Agent, however the bonding force at three kinds of substances, 2 interfaces can not " dynamic equilibrium ", it is viscous with transition zone since abrasive blasting is processed
Relay is big, so often resulting in multiple material and transition zone unsticking.The present invention for starting point, is increased another modified with " dynamic equilibrium "
Adhesive, wherein " compatibility " and ontology phenolic aldehyde of nbr carboxyl terminal filler and sheet rubber and " compatibility " of multiple material improve
The bonding force of transition zone sheet rubber and multiple material, it is sufficient to and another interfacial bonding dynamic balance, therefore ensure that interface bond quality.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair
Bright technical solution is clearly and completely described.Obviously, described embodiment is a part of the embodiments of the present invention, and
The embodiment being not all of.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative work
Under the premise of every other embodiment obtained, shall fall within the protection scope of the present invention.
The present invention provides a kind of phenolic resin preimpregnation material and metalwork integral formation method, the method in first aspect
Include:
(1) the pretreated step of metalwork: blast processing is carried out to the type face that metalwork needs to be bonded, then in metal mold
Brushwork gelatin on face.The type face being bonded can also be needed to be wiped with alcohol or acetone metalwork before carrying out blast processing
Only.It carries out that the surface alcohol or acetone wiped clean of sand can will have been blown after blast processing, brushwork gelatin again after drying.Institute
Can stating glue select?.
(2) the compound transition zone on through step (1) treated type face the step of.The step specifically includes:
(21) the step of preparing transition zone.The transition zone is preferably 9621 nitrile rubber transition zones, can be in form
9621 nitrile rubber pieces.The step can be carried out as follows: being divided the type face region of metallic object, cut out 9621 butyronitrile rubbers
The size of glue, with acetone by 9621 nitrile rubber wiped cleans.(22) the step of adhesive transition layer.The step can be according to as follows
Mode carries out: then the brushwork gelatin on the type face of 9621 nitrile rubbers and metallic object respectively is successively glued according to the region of segmentation
It connects on metallic object.Here glue can be epoxies glue, such as epoxy resin solution.
(23) vulcanize the step of, the vulcanization preferably carries out at 90-95 DEG C, for example, can be 90 DEG C, 91 DEG C, 92 DEG C,
93 DEG C, 94 DEG C, 95 DEG C, preferably vulcanize 2-2.5h at such a temperature.
(3) the step of material carries out laying: the brushing phenolic resin on the type face for be compounded with transition zone is presoaked to phenolic resin
Adhesive, then by phenolic resin preimpregnation material according to designed ply stacking-sequence and thickness laying；The phenolic resin adhesive
Include 100 parts by weight of phenolic resin, nbr carboxyl terminal 100-120 parts by weight, dispersing agent 0.5-1 parts by weight, if phenolic aldehyde tree
Rouge accounting is too big, and glue solidification can be more crisp；If nbr carboxyl terminal accounting is excessive, glue is too sticky, influences craftsmanship.Point
Powder can be polyvinyl alcohol and/or polypyrrole alkanone.
(4) the step of solidifying.Present invention preferably employs solidification of hot-press tank methods to be solidified, the solidification of hot-press tank method according to
Following method carries out:
It is warming up to 90-100 DEG C, pressurize 0.5MPa, keeps the temperature 1-1.5h；
It is warming up to 115-125 DEG C, pressurize 0.8MPa, keeps the temperature 2-2.5h；
It is warming up to 155-165 DEG C, keeps the temperature 4-4.5h；
Stop heating, it is with pressure be cooled to 60 DEG C hereinafter, rate of pressure reduction less than 2 DEG C/min.
It can also include after solidification mach step: three-dimensional digital-to-analogue being carried out to the product outer profile after solidification and is added
Work.
It is the embodiment that the present invention enumerates below.
Embodiment 1
Certain engineering complex profile aircraft (cabin) outer solar heat protection is prepared, integrated forming technique includes the following steps:
1. cabin pre-processes: the metal covering alcohol wipe for needing to be bonded is clean, then carry out blast processing.Sand is blown
Surface scrubbed with alcohol, waiting dry after, brushing first pass epoxy resin adhesive liquid；
2. nitrile rubber transition zone prepares: segmentation cabin type face region is cut out and comparable 9621 fourth of molding surface size in advance
Nitrile rubber, with the positive and negative wiped clean of acetone, for use；
3. rubber is bonding with cabin: the brushwork gelatin on sheet rubber and cabin blast type face respectively, then according to preparatory
The region divided successively is bonded in cabin, handles seam region well, then vacuumizes the presulfurization 2h in 90 DEG C of baking oven；
4. prepreg overlay: cabin external coating synvaren after step 3, synvaren are matched
Side are as follows: then 100 parts by weight of phenolic resin, 100 parts by weight of nbr carboxyl terminal, 0.5 parts by weight of polyethylene of dispersing agent alcohol are pressed
According to designed ply stacking-sequence and thickness laying；
5. solidification of hot-press tank: it is to be solidified that product after step 4 being vacuumized push-in autoclave etc..Program curing is as follows: room
Temperature --- starts to warm up (fixed 90 DEG C of temperature) --- 90 DEG C --- pressurization 0.5MPa, keeps the temperature 1h --- heating (fixed 120 DEG C of temperature) ---
120 DEG C --- pressurization 0.8MPa, keeping the temperature 2h, --- heating (fixed 160 DEG C of temperature) --- 160 --- keeps the temperature 4h, Guan Jiare, band pressure drop
Temperature goes out tank to 60 DEG C or less (rate of temperature fall is less than 2 DEG C/min)；
6. machining: carrying out three-dimensional digital-to-analogue processing to the product outer profile of integrated curing molding, formal part is obtained after processing and is produced
Product.
Reference standard GJB 1038.1A-2004 ultrasonic inspection, using NDTS-90 analog machine test, set dB value as
45, unsticking region is not found in probe accuracy rating.
Embodiment 2
Certain engineering complex profile aircraft (cabin) outer solar heat protection is prepared, integrated forming technique includes the following steps:
1. cabin pre-processes: the metal covering alcohol wipe for needing to be bonded is clean, then carry out blast processing.Sand is blown
Surface scrubbed with alcohol, it is stand-by every other day after drying；
2. nitrile rubber transition zone prepares: segmentation cabin type face region is cut out and comparable 9621 fourth of molding surface size in advance
Nitrile rubber, with the positive and negative wiped clean of acetone, for use；
3. rubber is bonding with cabin: the brushwork gelatin on sheet rubber and cabin blast type face respectively, then according to preparatory
The region divided successively is bonded in cabin, handles seam region well, then vacuumizes the presulfurization 2h in 90 DEG C of baking oven；
4. prepreg overlay: cabin external coating synvaren after step 3, synvaren are matched
Side are as follows: then 100 parts by weight of phenolic resin, 100 parts by weight of nbr carboxyl terminal, 0.5 parts by weight of polyethylene of dispersing agent alcohol are pressed
According to designed ply stacking-sequence and thickness laying；
5. solidification of hot-press tank: it is to be solidified that product after step 4 being vacuumized push-in autoclave etc..Program curing is as follows: room
Temperature --- starts to warm up (fixed 90 DEG C of temperature) --- 190 DEG C --- pressurization 0.5MPa, keeps the temperature 1h --- heating (fixed 120 DEG C of temperature) ---
--- 160 DEG C --- of 120 DEG C --- pressurization 0.8MPa, keep the temperature 2h --- heatings (fixed 160 DEG C of temperature) heat preservation 4h, Guan Jiare, it is with pressure
It is cooled to 60 DEG C or less (rate of temperature fall is less than 2 DEG C/min) and goes out tank；
6. machining: carrying out three-dimensional digital-to-analogue processing to the product outer profile of integrated curing molding, formal part is obtained after processing and is produced
Product.
Reference standard GJB 1038.1A-2004 ultrasonic inspection, using NDTS-90 analog machine test, set dB value as
45, in probe accuracy rating, measure region unsticking at 3, area is 5cm × 7.5cm, 4.5cm × 8cm, 12cm ×
3.5cm is metal cabin and rubber transition zone unsticking.
Embodiment 3
Certain engineering complex profile aircraft (cabin) outer solar heat protection is prepared, integrated forming technique includes the following steps:
1. cabin pre-processes: then the metal covering acetone wiped clean that needs are bonded carries out blast processing.Sand is blown
Surface scrubbed immediately with acetone, waiting dry after, brushing first pass epoxy resin adhesive liquid；
2. nitrile rubber transition zone prepares: segmentation cabin type face region is cut out and comparable 9621 fourth of molding surface size in advance
Nitrile rubber, with the positive and negative wiped clean of acetone, for use；
3. rubber is bonding with cabin: the brushwork gelatin on sheet rubber and cabin blast type face respectively, then according to preparatory
The region divided successively is bonded in cabin, handles seam region well, then vacuumizes the presulfurization 2h in 90 DEG C of baking oven；
4. prepreg overlay: cabin surface after step 3 is according to designed ply stacking-sequence and thickness laying；
5. solidification of hot-press tank: it is to be solidified that product after step 4 being vacuumized push-in autoclave etc..Program curing is as follows: room
Temperature --- starts to warm up (fixed 90 DEG C of temperature) --- 90 DEG C --- pressurization 0.5MPa, keeps the temperature 1h --- heating (fixed 120 DEG C of temperature) ---
--- 160 DEG C --- of 120 DEG C --- pressurization 0.8MPa, keep the temperature 2h --- heatings (fixed 160 DEG C of temperature) heat preservation 4h, Guan Jiare, it is with pressure
It is cooled to 60 DEG C or less (rate of temperature fall is less than 2 DEG C/min) and goes out tank；
6. machining: carrying out three-dimensional digital-to-analogue processing to the product outer profile of integrated curing molding, formal part is obtained after processing and is produced
Product.
Reference standard GJB 1038.1A-2004 ultrasonic inspection, using NDTS-90 analog machine test, set dB value as
45, probe accuracy rating in, survey 4 at defect area, area be 2.5cm × 4cm, 3cm × 5.5cm, 4.5cm × 7cm,
10cm × 3.5cm is transition zone and multiple material unsticking.
Embodiment 4
Certain engineering complex profile aircraft (cabin) outer solar heat protection is prepared, integrated forming technique includes the following steps:
1. cabin pre-processes: the metal covering alcohol wipe for needing to be bonded is clean, then carry out blast processing.Sand is blown
Surface scrubbed with alcohol, waiting dry after, brushing first pass glue；
2. nitrile rubber transition zone prepares: segmentation cabin type face region cuts out size and comparable 9621 fourth in type face in advance
Nitrile rubber, with the positive and negative wiped clean of acetone, for use；
3. rubber is bonding with cabin: the brushwork gelatin on sheet rubber and cabin blast type face respectively, then according to preparatory
The region divided successively is bonded in cabin, handles seam region well, then vacuumizes the presulfurization 2h in 90 DEG C of baking oven；
4. prepreg overlay: cabin external coating glue of the same race after step 3, then according to designed ply stacking-sequence
With thickness laying；
5. solidification of hot-press tank: it is to be solidified that product after step 4 being vacuumized push-in autoclave etc..Program curing is as follows: room
Temperature --- starts to warm up (fixed 90 DEG C of temperature) --- 9 DEG C --- pressurization 0.5MPa, keeps the temperature 1h --- heating (fixed 120 DEG C of temperature) ---
--- 160 DEG C 9 --- of 120 DEG C 9 --- pressurization 0.8MPa, keep the temperature 2h --- heating (fixed 160 DEG C of temperature) heat preservation 4h, Guan Jiare, band
Pressure is cooled to 60 DEG C or less (rate of temperature fall is less than 2 DEG C/min) and goes out tank；
6. machining: carrying out three-dimensional digital-to-analogue processing to the product outer profile of integrated curing molding, formal part is obtained after processing and is produced
Product.
Reference standard GJB 1038.1A-2004 ultrasonic inspection, using NDTS-90 analog machine test, set dB value as
45, probe accuracy rating in, survey 2 at defect area, area be 3cm × 4.5cm, 7cm × 5.5cm, be transition zone
With multiple material unsticking.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features；
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (10)
1. a kind of phenolic resin preimpregnation material and metalwork integral formation method characterized by comprising
(1) the pretreated step of metalwork: blast processing is carried out to the type face that metalwork needs to be bonded, then on metal mold face
Brushwork gelatin；
(2) the compound transition zone on through step (1) treated type face the step of；
(3) the step of material carries out laying: the brushing phenolic resin gluing on the type face for be compounded with transition zone is presoaked to phenolic resin
Agent, then by phenolic resin preimpregnation material according to designed ply stacking-sequence and thickness laying；The phenolic resin adhesive includes
100 parts by weight of phenolic resin, nbr carboxyl terminal 100-120 parts by weight, dispersing agent 0.5-1 parts by weight；
(4) the step of solidifying.
2. the method according to claim 1, wherein
Solidified using solidification of hot-press tank method.
3. according to the method described in claim 2, it is characterized in that,
The solidification of hot-press tank method carries out as follows:
It is warming up to 90-100 DEG C, pressurize 0.5MPa, keeps the temperature 1-1.5h；
It is warming up to 115-125 DEG C, pressurize 0.8MPa, keeps the temperature 2-2.5h；
It is warming up to 155-165 DEG C, keeps the temperature 4-4.5h；
Stop heating, it is with pressure be cooled to 60 DEG C hereinafter, rate of pressure reduction less than 2 DEG C/min.
4. the method according to claim 1, wherein
The step (2) includes: the step of preparing transition zone；The step of adhesive transition layer；The step of with vulcanization.
5. according to the method described in claim 4, it is characterized in that,
The transition zone is 9621 nitrile rubber transition zones.
6. according to the method described in claim 5, it is characterized in that,
Vulcanized at 90-95 DEG C, vulcanization time is preferably 2-2.5h.
7. according to the method described in claim 5, it is characterized in that,
Described the step of preparing transition zone includes: the type face region for dividing metallic object, the size of 9621 nitrile rubbers is cut out, with third
Ketone is by 9621 nitrile rubber wiped cleans.
8. the method according to the description of claim 7 is characterized in that
The step of adhesive transition layer includes: the brushwork gelatin on the type face of 9621 nitrile rubbers and metallic object respectively, then
It is successively bonded on metallic object according to the region of segmentation.
9. the method according to claim 1, wherein
The dispersing agent is selected from polyvinyl alcohol and/or polypyrrole alkanone.
10. the method according to claim 1, wherein
After solidification further include mach step: three-dimensional digital-to-analogue processing is carried out to the product outer profile after solidification.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113930199A (en) * | 2021-11-12 | 2022-01-14 | 航天特种材料及工艺技术研究所 | Toughened phenolic adhesive and preparation method and application thereof |
| CN114571649A (en) * | 2022-03-11 | 2022-06-03 | 北京玻钢院复合材料有限公司 | Rapid pressing method for integrally formed heat-proof product with large length-diameter ratio heat-proof layer and metal piece for aerospace vehicle and product thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113930199A (en) * | 2021-11-12 | 2022-01-14 | 航天特种材料及工艺技术研究所 | Toughened phenolic adhesive and preparation method and application thereof |
| CN113930199B (en) * | 2021-11-12 | 2024-02-20 | 航天特种材料及工艺技术研究所 | Toughening phenolic adhesive and preparation method and application thereof |
| CN114571649A (en) * | 2022-03-11 | 2022-06-03 | 北京玻钢院复合材料有限公司 | Rapid pressing method for integrally formed heat-proof product with large length-diameter ratio heat-proof layer and metal piece for aerospace vehicle and product thereof |
| CN114571649B (en) * | 2022-03-11 | 2024-03-08 | 北京玻钢院复合材料有限公司 | Method for rapidly pressing heat-proof product formed by integrally forming heat-proof layer with metal piece and large length-diameter ratio for aerospace vehicle and heat-proof product formed by integrally forming heat-proof layer with metal piece |
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