CN117565416B - Method for preparing adhesive structure by adopting secondary adhesive process and composite adhesive structure - Google Patents
Method for preparing adhesive structure by adopting secondary adhesive process and composite adhesive structure Download PDFInfo
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- CN117565416B CN117565416B CN202410054991.5A CN202410054991A CN117565416B CN 117565416 B CN117565416 B CN 117565416B CN 202410054991 A CN202410054991 A CN 202410054991A CN 117565416 B CN117565416 B CN 117565416B
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- 238000000034 method Methods 0.000 title claims abstract description 118
- 230000008569 process Effects 0.000 title claims abstract description 66
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 239000000853 adhesive Substances 0.000 title claims description 9
- 230000001070 adhesive effect Effects 0.000 title claims description 9
- 239000002313 adhesive film Substances 0.000 claims abstract description 74
- 238000004806 packaging method and process Methods 0.000 claims abstract description 41
- 238000012795 verification Methods 0.000 claims abstract description 24
- 238000004026 adhesive bonding Methods 0.000 claims description 44
- 239000003292 glue Substances 0.000 claims description 43
- 239000003822 epoxy resin Substances 0.000 claims description 32
- 229920000647 polyepoxide Polymers 0.000 claims description 32
- 239000002202 Polyethylene glycol Substances 0.000 claims description 29
- 229920001223 polyethylene glycol Polymers 0.000 claims description 29
- 238000001816 cooling Methods 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 12
- 239000012745 toughening agent Substances 0.000 claims description 12
- 239000004202 carbamide Substances 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 11
- 230000004888 barrier function Effects 0.000 claims description 10
- 239000004695 Polyether sulfone Substances 0.000 claims description 9
- 229920006393 polyether sulfone Polymers 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 8
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000012945 sealing adhesive Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 229920000459 Nitrile rubber Polymers 0.000 claims description 3
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- 230000001360 synchronised effect Effects 0.000 claims description 3
- 229920001169 thermoplastic Polymers 0.000 claims description 3
- 239000004416 thermosoftening plastic Substances 0.000 claims description 3
- 150000003672 ureas Chemical class 0.000 claims description 3
- 241000381602 Vachellia nebrownii Species 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000003825 pressing Methods 0.000 description 6
- 230000007704 transition Effects 0.000 description 6
- 239000012790 adhesive layer Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 238000002955 isolation Methods 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 5
- 229920001971 elastomer Polymers 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000007788 roughening Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000000712 assembly Effects 0.000 description 2
- 238000000429 assembly Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 239000011157 advanced composite material Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229920006332 epoxy adhesive Polymers 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000009659 non-destructive testing Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000009516 primary packaging Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
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Classifications
-
- 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
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
- B29C65/50—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding using adhesive tape, e.g. thermoplastic tape; using threads or the like
-
- 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
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/78—Means for handling the parts to be joined, e.g. for making containers or hollow articles, e.g. means for handling sheets, plates, web-like materials, tubular articles, hollow articles or elements to be joined therewith; Means for discharging the joined articles from the joining apparatus
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Lining Or Joining Of Plastics Or The Like (AREA)
Abstract
The invention provides a method for preparing a bonding structure by adopting a secondary bonding process and a composite bonding structure, belonging to the technical field of composite material connection. The method comprises the following steps: providing a first product, a second product and an adhesive film; providing a first vacuum bag assembly, and packaging the first workpiece, the second workpiece, the adhesive film and the first vacuum bag assembly according to a preset first packaging method to obtain a packaging piece to be verified; placing the packaging piece to be verified in an autoclave, and verifying according to a preset verification process to obtain a verified adhesive film; providing a second vacuum bag assembly, and packaging the first workpiece, the second workpiece, the checked adhesive film and the second vacuum bag assembly according to a preset second packaging method to obtain a packaging piece to be solidified; and placing the packaging piece to be cured in an autoclave, and curing according to a preset curing process to obtain a cementing structure. The method provided by the invention can solve the bonding defect caused by the fit clearance of the bonding surface which is easy to be wrapped by air and is in secondary bonding process.
Description
Technical Field
The invention belongs to the technical field of composite material connection, and particularly relates to a method for preparing a glue joint structure by adopting a secondary glue joint process and a composite material glue joint structure.
Background
On modern aviation aircrafts, advanced composite materials are applied in a large amount, and the connection technology between different composite material parts is an important research object of composite material structures and processes.
The composite material part connection mode comprises co-curing gluing, co-gluing, secondary gluing and mechanical connection, and takes a reinforced wallboard structure as an example, the co-curing gluing process is to cure and form the reinforcing ribs and the skin together, the gluing quality of the co-curing process is good, the strength is high, but the problem of insufficient pressure transmission of local parts easily occurs at the connection part, and the co-gluing die structure is complex, so that the overall qualification rate is low. The co-cementing process is to cure one part, then wet-lay the other part and co-cementing the cured part to form, the co-cementing process has better forming quality, but the later formed wet part has larger forming quality risk, and the part formed first undergoes two thermal processes, and the secondary curing brings risk to the quality of the part. The mechanical connection needs to be assembled with a large number of fasteners, has high weight cost and low cost performance, and is generally applied to complex assembly structures which cannot be glued in the process. The secondary gluing process is to form two parts separately, glue the assembly surface of the two parts with glue film, and the two parts are cured and formed separately to form the part with high quality and high yield, and is limited by the complex precision of the parts and the large area glue adhering and gas wrapping and other comprehensive factors.
Disclosure of Invention
The invention aims to provide a method for solving the technical problems of easiness in air wrapping and poor bonding quality in a secondary bonding process by adopting extremely narrow phase transition temperature adhesive film matching process control.
In order to achieve the above object, the present invention provides a method for preparing a bonded structure by a secondary bonding process, the bonded structure being a composite bonded structure, the method comprising the steps of:
(1) Providing a first part, a second part and a glue film which are prepared from a composite material, wherein the glue film is a polyethylene glycol modified epoxy resin glue film which is pure solid at a temperature below 40 ℃ and liquid at a temperature above 50 ℃;
(2) Providing a first vacuum bag assembly, and packaging the first workpiece, the second workpiece, the adhesive film and the first vacuum bag assembly according to a preset first packaging method to obtain a packaging piece to be verified, wherein the first packaging method comprises the following steps: the adhesive film is clamped between the first workpiece and the second workpiece;
(3) Placing the packaging piece to be verified in an autoclave, and verifying according to a preset verification process to obtain a verified adhesive film, wherein the verification is used for changing the shape of the adhesive film so as to enable the lower surface of the adhesive film to be matched with the adhesive bonding surface of the first product and the upper surface of the adhesive film to be matched with the adhesive bonding surface of the second product;
(4) Providing a second vacuum bag assembly, and packaging the first workpiece, the second workpiece, the checked adhesive film and the second vacuum bag assembly according to a preset second packaging method to obtain a package to be solidified, wherein the second packaging method comprises the following steps: abutting the lower surface of the calibrated adhesive film with the adhesive bonding surface of the first workpiece, and abutting the upper surface of the calibrated adhesive film with the adhesive bonding surface of the second workpiece;
(5) And placing the packaging piece to be cured in an autoclave, and curing according to a preset curing process to obtain the adhesive joint structure.
In a specific embodiment, the preset verification process includes: heating to 50deg.C at a heating rate of 1deg.C/min, maintaining at 50deg.C for 30min, cooling to 30deg.C, discharging from autoclave, and the program operation in the autoclave starts to pressurize by 0.2Mpa and synchronously discharges the vacuum in the vacuum bag.
In a specific embodiment, the preset curing process includes: firstly, vacuumizing a vacuum bag, detecting leakage, starting a program, discharging vacuum after the lowest thermocouple is heated to 55 ℃, pressurizing to 0.7Mpa in a synchronous autoclave, heating to 150 ℃, preserving heat at 150 ℃ for 180min, and then cooling and discharging out of the autoclave.
In a specific embodiment, the polyethylene glycol modified epoxy resin adhesive film comprises the following components in percentage by mass, based on 100% of the total weight of the polyethylene glycol modified epoxy resin adhesive film: 45-90% of epoxy resin, 2-20% of toughening agent, 5-20% of curing agent and 3-15% of viscosity regulator, wherein the epoxy resin is glycidyl ether epoxy resin, the toughening agent is thermoplastic blending toughening agent, the curing agent is latent dicyandiamide curing agent matched with substituted urea accelerator, and the viscosity regulator is polyethylene glycol.
In a specific embodiment, the epoxy resin is bisphenol A epoxy resin, the polymerization degree is 30-300, the softening point is 50-90 ℃, and the toughening agent is selected from nitrile rubber particles or polyether sulfone particles.
In a specific embodiment, the polyethylene glycol modified epoxy resin adhesive film comprises the following components in percentage by mass: 75.2% of bisphenol A epoxy resin, 10% of 500-mesh polyethersulfone particles, 4% of dicyandiamide, 0.8% of organic urea accelerator and 10% of polyethylene glycol, wherein the average molecular weight of the bisphenol A epoxy resin is 18000, and the average molecular weight of the polyethylene glycol is 8000.
In a specific embodiment, the first vacuum bag assembly comprises a first vacuum bag, a first airfelt, a first non-porous barrier film, a hydroentangled felt, a porous barrier film, a first tooling and a first sealing adhesive tape, and the first packaging method specifically comprises: from bottom to top, tiling in proper order first frock, first finished piece, glued membrane, foraminiferous barrier film, water thorn felt, second finished piece, first no hole barrier film and first ventilated felt, then encapsulate with first vacuum bag and first joint strip.
In a specific embodiment, the second vacuum bag assembly includes a second vacuum bag, a second airfelt, a second non-porous barrier film, a second tooling, and a second sealing strip, and the second encapsulation method specifically includes: from bottom to top, tiling second frock, first finished piece, glued membrane after the verification, second finished piece, second imperforate barrier film and second airfelt in proper order, then encapsulate with second vacuum bag and second joint strip.
In a specific embodiment, step (6) is further included between step (3) and step (4), where step (6) specifically includes: and checking the matching condition of the checked adhesive film and the first and second workpieces, and when the matching condition meets the preset requirement, locally compensating the checked adhesive film.
The invention also provides a composite material adhesive bonding structure, which comprises a first workpiece and a second workpiece which are prepared from a composite material, and adhesive films with two sides respectively connected with the first workpiece and the second workpiece, wherein the composite material adhesive bonding structure is prepared by adopting the method.
The beneficial effects of the invention at least comprise:
1. the secondary gluing process provided by the invention adopts polyethylene glycol modified epoxy resin adhesive film with phase transition of 40-50 ℃, and sequentially carries out four procedures of primary packaging, verification, secondary packaging and solidification, in the verification procedure, the verification process parameters are controlled to enable the adhesive film to be converted into liquid state from solid state so as to enable the shape of two surfaces of the adhesive film to be more matched with the gluing surface of the first workpiece and the gluing surface of the second workpiece, and the fit clearance is reduced, so that the verified adhesive film is clamped between the gluing surface of the first workpiece and the gluing surface of the second workpiece for solidification, the technical problems of gluing pores, debonding and the like in the prior art can be solved, and the secondary gluing process has better gluing quality.
2. The traditional epoxy adhesive film adopts rubber elastomer copolymerization or melt mixing modification, has wider molecular weight distribution, is generally sticky at room temperature, has fluidity at more than 80 ℃, completes solid, viscous and liquid phase transition at more than 50 ℃ and even more, has tackiness at room temperature, is easy to wrap air on a cementing surface during cementing, has general fluidity at high temperature, and is not beneficial to exhausting air on the cementing surface. According to the invention, the polyethylene glycol modified epoxy resin adhesive film with obvious solid-liquid phase change is firstly selected, and the adhesive layer is subjected to solid-liquid phase change in the temperature range of 40-50 ℃ (about 10 ℃), so that on one hand, the risk of gas wrapping of a cementing layer under the room temperature operation condition can be greatly reduced; on the other hand, the compensation quality in verification can be greatly improved, and the quality risk of insufficient glue solution compensation in part solidification is reduced.
3. The curing process provided by the invention adopts the steps of vacuumizing when the glue film is in a solid state at room temperature, pressing and vacuumizing again when the temperature of the workpiece exceeds 50 ℃ and the interface is immersed by the glue layer, and vacuumizing the air at the fit gap of the workpiece in the solid state environment of the glue layer, so that the vacuum is discharged in the molten state of the glue film, the pressure of an autoclave is increased, the trace small molecules in the glue layer can be ensured to be crushed and fused into the glue solution, and the risk of curing and air wrapping of the glue layer in the secondary glue bonding process is effectively solved.
In addition to the objects, features and advantages described above, the present invention has other objects, features and advantages. The present invention will be described in further detail with reference to the drawings.
Drawings
FIG. 1 is a schematic flow chart of steps of a method for preparing a composite material bonded structure by a secondary bonding process according to an embodiment of the present invention;
FIG. 2 is a schematic diagram showing placement of the package to be verified provided in step S102 shown in FIG. 1;
FIG. 3 is a diagram showing the process parameters of the preset verification process in step S103 shown in FIG. 1;
FIG. 4 is a schematic layout diagram of the package to be cured provided in step S104 shown in FIG. 1;
FIG. 5 is a diagram showing the process parameters of the preset curing process of step S105 shown in FIG. 1;
FIG. 6 is a graph showing the viscosity-temperature profile of the adhesive film prepared in example 1;
FIG. 7 is a graph comparing a first bonded panel prepared in example 1 with a second bonded panel prepared in comparative example 1;
FIG. 8 is a graph showing the results of an ultrasonic A-scan test of a first bonded panel prepared in example 1;
fig. 9 is a metallographic micrograph of the subbing layer of the first bonded panel prepared in example 1.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Referring to fig. 1 to 5, the present invention provides a method for preparing a bonded structure by a secondary bonding process, wherein the bonded structure is a composite bonded structure, and the method comprises the following steps:
step S101, providing a first product 10 and a second product 20 which are prepared from a composite material, and a glue film 30A, wherein the glue film is a polyethylene glycol modified epoxy resin glue film which is pure solid at a temperature below 40 ℃ and liquid at a temperature above 50 ℃.
In the present invention, the first part 10 and the second part 20 are formed by a forming process separately, and then are bonded by a secondary bonding process provided by the present invention.
In this step, the first article and the second article are both pretreated articles, and the pretreatment method of the first article and the second article includes: and coarsening the glued joint surfaces of the first workpiece and the second workpiece respectively, and then cleaning with acetone, and dehumidifying at 105 ℃ for later use.
In this embodiment, the purpose of roughening the bonding surfaces of the first and second articles is to increase the bonding strength by increasing the rough strength of the surfaces.
In the invention, the roughening process is provided by the prior art, and the roughening process is not improved and can be used for roughening various surfaces such as polishing, sand blowing and the like.
The polyethylene glycol modified epoxy resin adhesive film provided by the invention is pure solid at the temperature below 40 ℃, has no viscosity to the touch, is liquid at the temperature exceeding 50 ℃, has better fluidity, and compared with the adhesive film in the prior art, has smaller phase transition interval, can complete solid-liquid phase transition of the adhesive layer at the temperature of 40-50 ℃ (about 10 ℃), and can greatly reduce the risk of air wrapping of an adhesive layer under the room temperature operation condition.
Preferably, the polyethylene glycol modified epoxy resin adhesive film comprises the following components in percentage by mass based on 100% of the total weight of the polyethylene glycol modified epoxy resin adhesive film: 45-90% of epoxy resin, 2-20% of toughening agent, 5-20% of curing agent and 3-15% of viscosity regulator, wherein the epoxy resin is glycidyl ether epoxy resin, the toughening agent is thermoplastic blending toughening agent, the curing agent is latent dicyandiamide curing agent matched with substituted urea accelerator, and the viscosity regulator is polyethylene glycol.
More preferably, the epoxy resin is bisphenol A epoxy resin, the polymerization degree is 30-300, the softening point is 50-90 ℃, the toughening agent is selected from nitrile rubber particles or polyether sulfone particles, and the curing agent comprises dicyandiamide and an organic urea accelerator.
More preferably, the polyethylene glycol modified epoxy resin adhesive film comprises the following components in percentage by mass: 75.2% of bisphenol A epoxy resin, 10% of 500-mesh polyethersulfone particles, 4% of dicyandiamide, 0.8% of organic urea accelerator and 10% of polyethylene glycol, wherein the average molecular weight of the bisphenol A epoxy resin is 18000, and the average molecular weight of the polyethylene glycol is 8000.
In the invention, the preparation method of the polyethylene glycol modified epoxy resin adhesive film specifically comprises the following steps: putting bisphenol A type epoxy resin and polyether sulfone particles into a reaction kettle, heating to 100 ℃, stirring for 60 minutes, cooling to 70 ℃, putting polyethylene glycol, dicyandiamide and an organic urea accelerator into the reaction kettle, rapidly stirring for 15 minutes, further cooling to below 60 ℃, taking out the reaction kettle, transferring the reaction kettle to a film pressing machine, and pressing a film at 60 ℃.
Step S102, providing a first vacuum bag assembly 40, and packaging the first part 10, the second part 20, the adhesive film 30A and the first vacuum bag assembly 40 according to a preset first packaging method to obtain a package to be verified, where the first packaging method includes: the adhesive film 30A is sandwiched between the first article 10 and the second article 20.
Referring to fig. 2, the first vacuum bag assembly 40 includes a first vacuum bag 41, a first airfelt 42, a first non-porous isolating membrane 43, a spunlaced felt 44, a porous isolating membrane 45, a first tooling 46 and a first sealing adhesive tape 47, and the first packaging method specifically comprises: the first tooling 46, the first product 10, the adhesive film 30A, the porous isolating film 45, the spunlaced mat 44, the second product 20, the first non-porous isolating film 43 and the first airfelt 42 are sequentially paved from bottom to top, and then the first tooling, the first product 10, the adhesive film 30A, the porous isolating film 45, the second product 20, the first non-porous isolating film 43 and the first airfelt 42 are packaged by the first vacuum bag 41 and the first sealing adhesive tape 47.
In the invention, the porous isolating film 45 is used for isolating the adhesive film and other parts on the adhesive film, the spunlaced felt is used for guiding air on the adhesive bonding surface, and the air on the adhesive bonding surface is rapidly guided away from the adhesive bonding interface by utilizing the characteristic of air guiding and glue impermeability of the spunlaced felt, so that the adhesive bonding surface is ensured not to be wrapped with air.
Step S103, placing the packaging piece to be verified in an autoclave, and verifying according to a preset verification process to obtain a verified adhesive film 30B, wherein the verification is used for changing the shape of the adhesive film so that the lower surface of the adhesive film is matched with the adhesive bonding surface of the first workpiece and the upper surface of the adhesive film is matched with the adhesive bonding surface of the second workpiece.
Referring to fig. 3, the preset verification process includes: the lowest even temperature of the thermocouple is controlled, the temperature is increased to 50 ℃ according to the heating rate of 1 ℃/min, the temperature is kept at 50 ℃ for 30min, the temperature is reduced to 30 ℃ and then the thermocouple is discharged out of the autoclave, and the program operation in the autoclave starts to pressurize by 0.2Mpa and synchronously discharges the vacuum in the vacuum bag.
It will be appreciated that this step also includes removing the first vacuum bag and other vacuum bag assemblies to provide separate first and second articles and a verified film.
In the verification procedure, a hole isolation film and a spunlaced felt are arranged between the adhesive film and the second workpiece, the adhesive bonding surface is not easy to wrap air, and the verification effect is good.
In this embodiment, the vacuum bag is evacuated to a pressure of 0.08-0.1 MPa.
In the step, the cooling can be carried out along with the cooling of the furnace or set with a cooling rate, and preferably, the cooling rate is 0.5-2 ℃/min.
Step S104, providing a second vacuum bag assembly 50, and packaging the first part 10, the second part 20, the film 30B after verification, and the second vacuum bag assembly 50 according to a preset second packaging method to obtain a package to be cured, where the second packaging method includes: and abutting the lower surface of the calibrated adhesive film 30B with the adhesive bonding surface of the first workpiece 10, and abutting the upper surface of the calibrated adhesive film 30B with the adhesive bonding surface of the second workpiece 20.
Referring to fig. 4, the second vacuum bag assembly 50 includes a second vacuum bag 51, a second airfelt 52, a second non-porous isolation film 53, a second tooling 54 and a second sealing adhesive tape 55, and the second packaging method specifically includes: the second tooling 54, the first manufactured piece 10, the film 30B after verification, the second manufactured piece 20, the second non-porous isolation film 53 and the second airfelt 52 are sequentially paved from bottom to top, and then the second vacuum bag 51 and the second sealing adhesive tape 55 are used for packaging.
In the present invention, the first vacuum bag assembly 40 and the second vacuum bag assembly 50 are named together with the first and second vacuum bag assemblies only to distinguish the checking process and the curing process, and the first vacuum bag, the second vacuum bag, the first airfelt, the second airfelt, the first non-porous isolation film, the second non-porous isolation film, the first tool and the second tool, and the first sealing rubber strip and the second sealing rubber strip can be reused as the same part during the actual operation.
And step 105, placing the packaging piece to be cured in an autoclave, and curing according to a preset curing process to obtain the adhesive structure.
Referring to fig. 5, the preset curing process includes: firstly, vacuumizing a vacuum bag, detecting leakage, starting a program, discharging vacuum after the lowest thermocouple is heated to 55 ℃, pressurizing to 0.7Mpa in a synchronous autoclave, heating to 150 ℃, preserving heat at 150 ℃ for 180min, and then cooling and discharging out of the autoclave.
In this embodiment, the vacuum bag is evacuated to 0.09-0.098 Mpa.
The cooling in this step can be cooling with the furnace or setting cooling rate.
The curing process provided by the invention adopts the steps of vacuumizing when the glue film is in a solid state at room temperature, pressing and vacuumizing again when the temperature of the workpiece exceeds 50 ℃ and the interface is immersed by the glue layer, and vacuumizing the air at the fit gap of the workpiece in the solid state environment of the glue layer, so that the vacuum is discharged in the molten state of the glue film, the pressure of an autoclave is increased, the trace small molecules in the glue layer can be ensured to be crushed and fused into the glue solution, and the risk of curing and air wrapping of the glue layer in the secondary glue bonding process is effectively solved.
Preferably, step S106 is further included between the step S103 and the step S104, and the step S106 is specifically: and checking the matching condition of the checked adhesive film and the first and second workpieces, and when the matching condition meets the preset requirement, locally compensating the checked adhesive film.
In this embodiment, the matching condition meets the preset requirement, which can be understood that a gap is formed between the adhesive bonding surface of the first workpiece and the lower surface of the adhesive film or between the adhesive bonding surface of the second workpiece and the upper surface of the adhesive film, and the compensation area is not large, in this case, the adhesive film needs to be locally compensated at the fit gap according to the actual condition, and the specific compensation method is as follows: and after the first workpiece and the second workpiece are matched, the first workpiece and the second workpiece are separated by a separation film, and the adhesive film is heated to more than 45 ℃ by using local simple heating equipment such as an electric iron or a blower, and is locally pressed and compacted manually.
The adhesive film can be changed from solid state to liquid state when being heated to 45 ℃, so that the secondary verification can be realized by directly and locally compensating for small defects, and the operation efficiency is high.
If the fit clearance is large and local compensation is not easy, the steps S102 and S103 are repeated, i.e. the verification process is repeated.
The invention also provides a composite material adhesive bonding structure, which comprises a first workpiece and a second workpiece which are prepared from a composite material, and adhesive films with two sides respectively connected with the first workpiece and the second workpiece, wherein the composite material adhesive bonding structure is prepared by adopting the method.
Example 1
The secondary cementing process provided by the invention is adopted to prepare a first cementing flat plate with the diameter of 300 mm 100mm
1.1 Preparation of an adhesive film
Firstly, preparing raw materials according to the following formula: bisphenol a type epoxy resin (average molecular weight 18000): 75.2%,500 mesh polyethersulfone particles: 10%, dicyandiamide: 4%, organic urea accelerator: 0.8%, polyethylene glycol (PEG-8000): 10%; then preparing a glue film, wherein the preparation method of the glue film comprises the following steps: putting bisphenol A type epoxy resin and polyether sulfone particles into a reaction kettle, heating to 100 ℃, stirring for 60 minutes to uniformly mix, then cooling to 70 ℃, putting polyethylene glycol, dicyandiamide and an organic urea accelerator into the reaction kettle, rapidly stirring for 15 minutes, further cooling to below 60 ℃, taking out the reaction kettle, transferring the reaction kettle to a film pressing machine, and pressing a film at 60 ℃.
The viscosity-temperature curve of the prepared adhesive film is shown in fig. 6, and it can be seen from the graph that the viscosity of the adhesive film rapidly decreases from 45 ℃, reaches 523pa.s at 50 ℃ and reaches the minimum viscosity 280Pa.s at 60 ℃, and the solid-liquid phase transition is completed within the temperature range of not more than 15 ℃.
1.2 The glass plate and the composite plate (the first workpiece and the second workpiece) are bonded by the secondary bonding process provided by the invention, the length and width dimensions of the glass plate and the composite plate are 300 mm by 100mm, and the first bonded plate 200 obtained by bonding is shown as a plate product on the left side of fig. 7.
The secondary bonding process of the present invention has been described in detail above and will not be described in detail in this section.
1.3 Nondestructive testing:
the first bonding plate is subjected to A-scan nondestructive test, the ultrasonic A-scan test result is shown in fig. 8, and obvious adhesive film interface waves and reflection bottom waves of the lower panel can be seen from ultrasonic waveforms, so that the bonding quality is good.
After the first bonding flat plate is cut, metallographic microstructure analysis is carried out, and the metallographic microscopic of the adhesive layer of the first bonding flat plate is shown in fig. 9, so that the first bonding flat plate manufactured by the method has compact adhesive layer without holes and good bonding quality as can be seen from a metallographic microscopic picture.
Comparative example 1
Preparation of a 300 x 100mm second glued plate using the prior art
The adhesive film adopted in comparative example 1 is a common J-116 adhesive film, the length and width dimensions of the glass flat plate and the composite flat plate are both 300 x 100mm, and the adhesive bonding method is similar to the invention, and the difference is that the adhesive film is different, so that the temperature parameters set by the verification process and the curing process are different, specifically, in the adhesive bonding method of comparative example, the verification process is heated to 70 ℃ for heat preservation treatment, and the curing process is heated to 175 ℃ for heat preservation treatment.
The second glue panel 300 prepared in the comparative example is shown in the panel product on the right side of fig. 7.
Referring to fig. 7, it can be seen from the product diagram on the right side of fig. 7 that the second bonding plate 300 prepared by using the common J-116 adhesive film and the common process parameters can see the obvious bonding failure caused by the air wrapping in the middle area 301 from the glass panel.
The foregoing is a further detailed description of the invention in connection with specific preferred embodiments, and is not intended to limit the practice of the invention to such description. It will be apparent to those skilled in the art that several simple deductions and substitutions can be made without departing from the spirit of the invention, and these are considered to be within the scope of the invention.
Claims (10)
1. A method for preparing a bonded structure by adopting a secondary bonding process, wherein the bonded structure is a composite bonded structure, and the method is characterized by comprising the following steps:
step (1), providing a first product and a second product which are prepared from a composite material, and a glue film, wherein the glue film is a polyethylene glycol modified epoxy resin glue film which is pure solid at a temperature below 40 ℃ and liquid at a temperature above 50 ℃;
step (2), providing a first vacuum bag assembly, and packaging the first workpiece, the second workpiece, the adhesive film and the first vacuum bag assembly according to a preset first packaging method to obtain a packaging piece to be verified, wherein the first packaging method comprises the following steps: the adhesive film is clamped between the first workpiece and the second workpiece;
step (3), placing the packaging piece to be verified in an autoclave, and verifying according to a preset verification process to obtain a verified adhesive film, wherein the verification is used for changing the shape of the adhesive film so as to enable the lower surface of the adhesive film to be matched with the adhesive bonding surface of the first workpiece and the upper surface of the adhesive film to be matched with the adhesive bonding surface of the second workpiece;
step (4), providing a second vacuum bag assembly, and packaging the first workpiece, the second workpiece, the checked adhesive film and the second vacuum bag assembly according to a preset second packaging method to obtain a packaging piece to be solidified, wherein the second packaging method comprises the following steps: abutting the lower surface of the calibrated adhesive film with the adhesive bonding surface of the first workpiece, and abutting the upper surface of the calibrated adhesive film with the adhesive bonding surface of the second workpiece;
and (5) placing the packaging piece to be cured in an autoclave, and curing according to a preset curing process to obtain the adhesive joint structure.
2. The method for manufacturing a bonded structure using a secondary bonding process according to claim 1, wherein the preset verification process comprises: heating to 50deg.C at a heating rate of 1deg.C/min, maintaining at 50deg.C for 30min, cooling to 30deg.C, discharging from autoclave, and the program operation in the autoclave starts to pressurize by 0.2Mpa and synchronously discharges the vacuum in the vacuum bag.
3. The method for preparing a bonded structure using a secondary bonding process according to claim 1, wherein the preset curing process comprises: firstly, vacuumizing a vacuum bag, detecting leakage, starting a program, discharging vacuum after the lowest thermocouple is heated to 55 ℃, pressurizing to 0.7Mpa in a synchronous autoclave, heating to 150 ℃, preserving heat at 150 ℃ for 180min, and then cooling and discharging out of the autoclave.
4. A method for preparing a glue joint structure by adopting a secondary glue joint process according to any one of claims 1 to 3, wherein the polyethylene glycol modified epoxy resin glue film comprises the following components in percentage by mass, based on 100% of the total weight of the polyethylene glycol modified epoxy resin glue film: 45-90% of epoxy resin, 2-20% of toughening agent, 5-20% of curing agent and 3-15% of viscosity regulator, wherein the epoxy resin is glycidyl ether epoxy resin, the toughening agent is thermoplastic blending toughening agent, the curing agent is latent dicyandiamide curing agent matched with substituted urea accelerator, and the viscosity regulator is polyethylene glycol.
5. The method for preparing a glue joint structure by adopting a secondary glue joint process according to claim 4, wherein the epoxy resin is bisphenol A type epoxy resin, the polymerization degree is 30-300, the softening point is 50-90 ℃, the toughening agent is nitrile rubber particles or polyether sulfone particles, and the curing agent comprises dicyandiamide and an organic urea accelerator.
6. The method for preparing a glue joint structure by adopting a secondary glue joint process according to claim 5, wherein the polyethylene glycol modified epoxy resin glue film comprises the following components in percentage by mass: 75.2% of bisphenol A epoxy resin, 10% of 500-mesh polyethersulfone particles, 4% of dicyandiamide, 0.8% of organic urea accelerator and 10% of polyethylene glycol, wherein the average molecular weight of the bisphenol A epoxy resin is 18000, and the average molecular weight of the polyethylene glycol is 8000.
7. The method for preparing a bonded structure by using a secondary bonding process according to claim 1, wherein the first vacuum bag component comprises a first vacuum bag, a first airfelt, a first non-porous isolating membrane, a spunlaced felt, a porous isolating membrane, a first tooling and a first sealing adhesive tape, and the first packaging method specifically comprises: from bottom to top, tiling in proper order first frock, first finished piece, glued membrane, foraminiferous barrier film, water thorn felt, second finished piece, first no hole barrier film and first air-felt, then encapsulate with first vacuum bag and first joint strip.
8. The method for preparing a bonded structure using a secondary bonding process according to claim 1 or 7, wherein the second vacuum bag assembly comprises a second vacuum bag, a second airfelt, a second non-porous barrier film, a second tooling and a second sealing strip, and the second packaging method specifically comprises: tiling in proper order from bottom to top second frock, first finished piece, glued membrane after the check, second finished piece, second imperforate barrier film and second airfelt, then encapsulate with second vacuum bag and second joint strip.
9. The method for preparing a bonded structure by using a secondary bonding process according to claim 1, wherein step (6) is further included between step (3) and step (4), and the step (6) specifically includes: and checking the matching condition of the checked adhesive film and the first and second workpieces, and when the matching condition meets the preset requirement, locally compensating the checked adhesive film.
10. A composite material adhesive bonding structure comprising a first part and a second part which are made of a composite material, and adhesive films with two sides respectively connected with the first part and the second part, wherein the composite material adhesive bonding structure is prepared by the method of any one of claims 1 to 9.
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| WO2013074265A1 (en) * | 2011-11-14 | 2013-05-23 | Henkel Corporation | Adhesive compositions |
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| US4070225A (en) * | 1976-11-17 | 1978-01-24 | H. B. Fuller Company | Method of using structural adhesive |
| CN103302952A (en) * | 2012-03-12 | 2013-09-18 | 日东电工株式会社 | Production method of flat panel display |
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