CN113861929A - Adhesive, preparation method thereof, low dielectric loss pure adhesive film applying adhesive and manufacturing process thereof - Google Patents
Adhesive, preparation method thereof, low dielectric loss pure adhesive film applying adhesive and manufacturing process thereof Download PDFInfo
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- 239000000853 adhesive Substances 0.000 title claims abstract description 77
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 77
- 239000002313 adhesive film Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 238000004519 manufacturing process Methods 0.000 title abstract description 13
- 229920000098 polyolefin Polymers 0.000 claims abstract description 27
- 239000004642 Polyimide Substances 0.000 claims abstract description 24
- 229920001721 polyimide Polymers 0.000 claims abstract description 24
- 229920013636 polyphenyl ether polymer Polymers 0.000 claims abstract description 23
- 239000000945 filler Substances 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims description 50
- 239000003292 glue Substances 0.000 claims description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 16
- 239000012790 adhesive layer Substances 0.000 claims description 14
- 239000010413 mother solution Substances 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 10
- 239000003822 epoxy resin Substances 0.000 claims description 10
- 229920000647 polyepoxide Polymers 0.000 claims description 10
- 239000004576 sand Substances 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 claims description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000012752 auxiliary agent Substances 0.000 claims description 6
- 229920002121 Hydroxyl-terminated polybutadiene Polymers 0.000 claims description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- 239000003963 antioxidant agent Substances 0.000 claims description 4
- 230000003078 antioxidant effect Effects 0.000 claims description 4
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 4
- 239000003063 flame retardant Substances 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 229920013638 modified polyphenyl ether Polymers 0.000 claims 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 11
- 229910000679 solder Inorganic materials 0.000 abstract description 8
- 125000003700 epoxy group Chemical group 0.000 abstract description 7
- 230000000052 comparative effect Effects 0.000 description 14
- 229920001955 polyphenylene ether Polymers 0.000 description 7
- 239000012452 mother liquor Substances 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000005062 Polybutadiene Substances 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000010365 information processing Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J179/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09J161/00 - C09J177/00
- C09J179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C09J179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/10—Adhesives in the form of films or foils without carriers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
Abstract
The invention provides an adhesive and a preparation method thereof, a low dielectric loss pure adhesive film applying the adhesive and a manufacturing process thereof, wherein the adhesive comprises 30-80 parts of modified polyimide, 10-30 parts of polyphenyl ether, 5-20 parts of epoxidized polyolefin and 30-80 parts of filler, the application uses the combination of the modified polyimide, the polyphenyl ether, the epoxidized polyolefin and the filler, the modified polyimide with low dielectric constant and low dielectric loss is selected, the selected polyphenyl ether does not contain other polar groups except hydroxyl groups at two ends, the selected epoxidized polyolefin does not contain other polar groups except the epoxy groups and the hydroxyl groups at two ends, as the polar groups are reduced in the components, the prepared pure adhesive film has very low dielectric loss and dielectric constant, and compared with the traditional pure adhesive film, the adhesive film has lower dielectric constant and dielectric loss on the basis of ensuring the original requirements, the high-temperature-resistant solder has the advantages of low dielectric loss and dielectric constant, and has excellent high-temperature-resistant solder heat resistance and peeling strength.
Description
Technical Field
The application relates to the technical field of pure glue films, in particular to an adhesive for a pure glue film and a preparation method thereof, and a low dielectric loss pure glue film using the adhesive and a manufacturing process thereof.
Background
In recent years, with rapid development of the electronic industry, information processing and information transmission speed is increased, and the performance requirements of circuit board materials are higher and higher, and the dielectric constant and dielectric loss of the antenna board materials in the circuit board materials are higher, because the higher the dielectric loss is, the higher the loss of signals in the transmission process is.
The pure glue film is mainly applied to a multilayer board and plays a role in bridge connection, and along with the continuous development of the 5G technology, the requirements on the dielectric constant and the dielectric loss of the pure glue film are lower and lower. However, since the conventional pure glue film has a relatively large number of polar groups therein, the dielectric constant and the dielectric loss thereof are relatively large, and the requirement of high frequency and high speed is not satisfied, it is urgently needed to provide a pure glue film with a lower dielectric constant and dielectric loss to satisfy the requirement of a high frequency and high speed circuit board.
Disclosure of Invention
In order to solve the technical problem that the dielectric constant and the dielectric loss of a pure adhesive film are large in the prior art, the application provides an adhesive with low dielectric loss and dielectric constant, a preparation method thereof, a low dielectric loss pure adhesive film using the adhesive and a manufacturing process thereof.
The adhesive comprises the following components in parts by weight: 30-80 parts of modified polyimide, 10-30 parts of polyphenyl ether, 5-20 parts of epoxidized polyolefin and 30-80 parts of filler, wherein the adhesive is prepared by using the combination of the modified polyimide, the polyphenyl ether, the epoxidized polyolefin and the filler, a modified polyimide solution with low dielectric constant and low dielectric loss is selected to serve as reaction main body resin and toughening effect in the components, the selected polyphenyl ether does not contain other polar groups except hydroxyl groups at two ends, the selected epoxidized polyolefin does not contain other polar groups except epoxy groups and hydroxyl groups at two ends, and the dielectric loss and the dielectric constant of the prepared adhesive are very low due to the reduction of the polar groups in the components. The high-temperature-resistant solder has the advantages of low dielectric loss and dielectric constant, and has excellent high-temperature-resistant solder heat resistance and peeling strength.
Preferably, the polyphenylene ether is modified polyphenylene ether SA-9000, SA-9000 has the characteristic of low dielectric property, and compared with the existing pure film component, the polyphenylene ether has more polar groups, so that the dielectric constant and the dielectric loss of the existing circuit board are larger, the polyphenylene ether used in the application has a symmetrical structure, and has no other polar groups except hydroxyl groups at two ends, so that the dielectric loss and the dielectric constant are both low, and the hydroxyl groups can also react with carboxyl/amino groups in a modified polyimide solution to reduce the dielectric loss and the dielectric constant of an adhesive system, and the molecular formula of the polyphenylene ether is as follows:
preferably, the epoxidized polyolefin is epoxidized hydroxyl terminated polybutadiene or dicyclopentadiene phenol epoxy resin, most of the components of the existing pure glue film use epoxy resin, and Df (dielectric loss) is obviously increased after the epoxy resin is added, which influences the Df (dielectric loss) value of the material mainly because the epoxy resin carries other polar groups such as-CH (carboxyl) besides epoxy group3Polar groups such as-0-, 0H, -CH (O) CH-, etc., which have a relatively high specific gravity and result in a relatively high dielectric property; the Df value of the epoxy resin can be effectively reduced by using the epoxy group with low dielectric value, and the epoxy groupThe selected epoxidized hydroxyl-terminated polybutadiene and dicyclopentadiene phenol epoxy resin can effectively improve the crosslinking density and heat resistance, other polar groups are basically absent except epoxy groups and hydroxyl groups at two ends, so that the dielectric property of the epoxy-terminated polybutadiene and dicyclopentadiene phenol epoxy resin is smaller, Dk and Df in a glue system can be effectively reduced, and the epoxy groups can easily react with other polar groups to generate a three-dimensional network structure polymer.
The molecular formula of the epoxidized hydroxyl-terminated polybutadiene is as follows:
the molecular formula of the dicyclopentadiene phenol epoxy resin is as follows:
preferably, the filler is silicon dioxide, and because the solubility of the modified polyimide solution is relatively poor, the non-polar filler, namely the silicon dioxide, is selected as the filler in the application, so that the dispersibility is good, and the silicon dioxide also has relatively low dielectric constant and dielectric loss.
Preferably, the coating further comprises 0-3 parts of an auxiliary agent according to needs, wherein the auxiliary agent is one or any combination of a silane coupling agent, a flame retardant, an accelerator and an antioxidant, and can be added according to specific needs to improve corresponding performances.
Preferably, the emulsion further comprises 10-30 parts of a solvent, wherein the solvent is at least one of Methyl Ethyl Ketone (MEK) or cyclohexanone, has good compatibility with other components and is used for adjusting viscosity.
A second object of the present application is to provide a method for preparing an adhesive, comprising the steps of:
step A: sequentially adding polyphenyl ether, filler and solvent into a stirring kettle, mixing and stirring, and then sanding by using a sand mill to prepare a mother solution;
and B: and adding the mother solution, the polyimide solution and the epoxidized polyolefin into a stirring kettle, continuously stirring, stirring for 2-4h, and uniformly mixing to prepare the adhesive.
The application provides a preparation method of an adhesive, wherein polyphenyl ether, filler and solvent are sequentially added into a stirring kettle, mixed and stirred, then a sand mill is used for sanding for 2-3 times to prepare a mother solution, then the mother solution, a polyimide solution, epoxidized polyolefin, an auxiliary agent and other components are added into the stirring kettle to be continuously stirred, and the mixture is uniformly stirred for 2-4 hours to prepare the adhesive.
The third purpose of the application is to provide a low dielectric loss pure glue film, which comprises a release film, an adhesive layer and release paper, wherein the release film, the adhesive layer and the release paper are sequentially arranged, and the adhesive layer is formed by the adhesive.
A fourth object of the present application is to provide a process for manufacturing a low dielectric loss pure adhesive film, comprising the following steps: coating an adhesive on a release film, drying the release film coated with the adhesive for 100-500 s at 120-180 ℃ by using an oven, pressing the release film coated with the adhesive surface with release paper at 50-100 ℃ after drying, and thus preparing the low dielectric loss pure adhesive film.
Compared with the prior art, the beneficial effects of this application are as follows:
the adhesive comprises 30-80 parts of modified polyimide, 10-30 parts of polyphenyl ether, 5-20 parts of epoxidized polyolefin and 30-80 parts of filler, wherein the combination of the modified polyimide, the polyphenyl ether, the epoxidized polyolefin and the filler is used, a modified polyimide solution with low dielectric constant and low dielectric loss is selected to serve as reaction main body resin and toughening effect in the components, the selected polyphenyl ether does not contain other polar groups except hydroxyl groups at two ends, the selected epoxidized polyolefin does not contain other polar groups except the epoxy group and the hydroxyl groups at two ends, and the prepared adhesive has low dielectric loss and dielectric constant due to the reduction of the polar groups in the components. The high-temperature-resistant solder has the advantages of low dielectric loss and dielectric constant, and has excellent high-temperature-resistant solder heat resistance and peeling strength.
The application provides a preparation method of an adhesive, wherein polyphenyl ether, filler and solvent are sequentially added into a stirring kettle, mixed and stirred, then a sand mill is used for sanding for 2-3 times to prepare a mother solution, then the mother solution, a polyimide solution, epoxidized polyolefin, an auxiliary agent and other components are added into the stirring kettle to be continuously stirred, and the mixture is uniformly stirred for 2-4 hours to prepare the adhesive.
The application provides a low dielectric loss pure glue film, which comprises a release film, an adhesive layer and release paper, wherein the release film, the adhesive layer and the release paper are sequentially arranged, the adhesive layer is an adhesive prepared from the combination of modified polyimide, polyphenyl ether, epoxidized polyolefin and a filler, and compared with the existing common pure glue film, the low dielectric loss pure glue film disclosed by the invention has lower dielectric constant and dielectric loss.
The application provides a manufacturing process of a low dielectric loss pure glue film, which comprises the following steps: the adhesive is coated on the release film, the release film coated with the adhesive is dried for 100-500 s at 120-180 ℃ by an oven, the release film coated with the adhesive surface is pressed with release paper at 50-100 ℃ after drying, and the prepared pure adhesive film has low dielectric constant and low dielectric loss after meeting the basic physical properties of the pure adhesive film, and can be applied to high-frequency high-speed circuit boards.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings used in the description of the embodiments will be briefly introduced below.
Fig. 1 is a schematic structural diagram of a pure adhesive film in an embodiment of the present application.
Detailed Description
The following describes a specific embodiment of the present invention with reference to specific examples 1 to 6 and comparative examples 1 to 3:
example 1:
a preparation method of the adhesive comprises the following steps:
weighing the components according to the weight parts in the table 1, sequentially adding polyphenyl ether, filler and solvent into a stirring kettle, mixing and stirring, and sanding for 2 times by using a sand mill after stirring to prepare mother liquor; and adding the mother solution, the polyimide solution and the epoxidized polyolefin into a stirring kettle, continuously stirring, stirring for 4 hours, and uniformly mixing to prepare the adhesive.
A manufacturing process of a low dielectric loss pure glue film comprises the following steps: and B, coating the adhesive prepared in the step B on a release film 1 to form an adhesive layer 2, drying the release film 1 coated with the adhesive for 300s at 160 ℃, and pressing the release film 1 coated with the adhesive surface with release paper 3 at 80 ℃ to prepare the low dielectric loss pure adhesive film shown in the figure 1.
Example 2:
a preparation method of the adhesive comprises the following steps:
weighing the components according to the weight parts in the table 1, sequentially adding polyphenyl ether, filler and solvent into a stirring kettle, mixing and stirring, and sanding for 3 times by using a sand mill after stirring to prepare mother liquor; and adding the mother solution, the polyimide solution and the epoxidized polyolefin into a stirring kettle, continuously stirring, stirring for 2 hours and uniformly mixing to prepare the adhesive.
A manufacturing process of a low dielectric loss pure glue film comprises the following steps: coating an adhesive on a release film 1 to form an adhesive layer 2, drying the release film 1 coated with the adhesive for 500s at 120 ℃ in an oven, and pressing the release film 1 coated with the adhesive with release paper 3 at 60 ℃ to prepare the low dielectric loss pure adhesive film shown in the figure 1.
Example 3:
a preparation method of the adhesive comprises the following steps:
weighing the components according to the weight parts in the table 1, sequentially adding polyphenyl ether, filler and solvent into a stirring kettle, mixing and stirring, and sanding for 2 times by using a sand mill after stirring to prepare mother liquor; and adding the mother solution, the polyimide solution and the epoxidized polyolefin into a stirring kettle, continuously stirring, stirring for 3 hours, and uniformly mixing to prepare the adhesive.
A manufacturing process of a low dielectric loss pure glue film comprises the following steps: coating an adhesive on a release film 1 to form an adhesive layer 2, drying the release film 1 coated with the adhesive for 100s at 180 ℃ in an oven, and pressing the release film 1 coated with the adhesive surface with release paper 3 at 90 ℃ to prepare the low dielectric loss pure adhesive film shown in the figure 1.
Example 4:
a preparation method of the adhesive comprises the following steps:
weighing the components according to the weight parts in the table 1, sequentially adding polyphenyl ether, filler and solvent into a stirring kettle, mixing and stirring, and sanding for 3 times by using a sand mill after stirring to prepare mother liquor; and adding the mother solution, the polyimide solution, the epoxidized polyolefin and the flame retardant into a stirring kettle, continuously stirring, stirring for 4 hours, and uniformly mixing to prepare the adhesive.
A manufacturing process of a low dielectric loss pure glue film comprises the following steps: coating an adhesive on a release film 1 to form an adhesive layer 2, drying the release film 1 coated with the adhesive for 400s at 150 ℃ in an oven, and pressing the release film 1 coated with the adhesive with release paper 3 at 70 ℃ to prepare the low dielectric loss pure adhesive film shown in the figure 1.
Example 5:
a preparation method of the adhesive comprises the following steps:
weighing the components according to the weight parts in the table 1, sequentially adding polyphenyl ether, filler and solvent into a stirring kettle, mixing and stirring, and sanding for 3 times by using a sand mill after stirring to prepare mother liquor; and adding the mother solution, the polyimide solution, the epoxidized polyolefin, the silane coupling agent and the antioxidant into a stirring kettle, continuously stirring, stirring for 4 hours, and uniformly mixing to prepare the adhesive.
A manufacturing process of a low dielectric loss pure glue film comprises the following steps: coating an adhesive on a release film 1 to form an adhesive layer 2, drying the release film 1 coated with the adhesive for 400s at 130 ℃ in an oven, and pressing the release film 1 coated with the adhesive with release paper 3 at 80 ℃ to prepare the low dielectric loss pure adhesive film shown in the figure 1.
Example 6:
a preparation method of the adhesive comprises the following steps:
weighing the components according to the weight parts in the table 1, sequentially adding polyphenyl ether, filler and solvent into a stirring kettle, mixing and stirring, and sanding for 2 times by using a sand mill after stirring to prepare mother liquor; and adding the mother solution, the polyimide solution, the epoxidized polyolefin, the silane coupling agent, the accelerator and the antioxidant into a stirring kettle, continuously stirring, stirring for 3 hours, and uniformly mixing to prepare the adhesive.
A manufacturing process of a low dielectric loss pure glue film comprises the following steps: coating an adhesive on a release film 1 to form an adhesive layer 2, drying the release film 1 coated with the adhesive for 150s at 170 ℃ in an oven, and pressing the release film 1 coated with the adhesive with release paper 3 at 100 ℃ to prepare the low dielectric loss pure adhesive film shown in the figure 1.
Comparative example 1:
the preparation procedure and components were the same as in comparative example 1 except that no epoxidized polyolefin was added to the components.
Comparative example 2:
the procedure and composition were the same as in comparative example 2, except that bisphenol A epoxy resin was used instead of the epoxidized polyolefin.
Comparative example 3:
the preparation procedure and components were the same as in comparative example 3 except that no polyphenylene ether was added to the components.
Table 1: weight proportion of adhesive in examples 1-6 and comparative examples 1-3
The pure adhesive films prepared in examples 1 to 6 and comparative examples 1 to 3 were subjected to comparative property tests, and the test items and test results are shown in table 2:
table 2: results of Performance test of pure adhesive films obtained in examples 1 to 6 and comparative examples 1 to 3
The test results in the experimental table 2 show that the dielectric constant of the pure adhesive film prepared by the method can reach below 2.9, the dielectric loss value can reach below 0.005, the stripping force and the soldering tin heat resistance are qualified, and the pure adhesive film has high heat resistance and high bonding force and can meet the performance requirements of the flexible printed circuit board of the high-frequency and high-speed electronic and electrical appliances; comparative example 1 no epoxidized polyolefin was added, resulting in both peel strength and solder heat resistance being unacceptable; comparative example 2 used a bisphenol A epoxy resin having a dielectric constant of 3.0 and a dielectric loss value of 0.0061, since the bisphenol A epoxy resin carries some other polar groups, such as-CH3Polar groups such as-0-, 0H, -CH (O) CH-, etc., which have a relatively high specific gravity and result in a relatively high dielectric property; the no addition of polyphenylene ether in the component of the comparative document 3 results in the poor solder heat resistance; the invention selects the modified polyimide solution with low dielectric constant and low dielectric loss to serve as reaction main body resin and toughening effect in the components, the selected polyphenyl ether does not contain other polar groups except hydroxyl groups at two ends, the selected epoxidized polyolefin does not contain other polar groups except epoxy groups and hydroxyl groups at two ends, and the prepared adhesive has very low dielectric loss and dielectric constant due to the fact that the polar groups are reduced in the components.
Claims (10)
1. The adhesive is characterized by comprising the following components in parts by weight: 30-80 parts of modified polyimide, 10-30 parts of polyphenyl ether, 5-20 parts of epoxidized polyolefin and 30-80 parts of filler.
2. The adhesive of claim 1, wherein: the polyphenyl ether is modified polyphenyl ether SA-9000.
3. The adhesive of claim 1, wherein: the epoxidized polyolefin is epoxidized hydroxyl terminated polybutadiene or dicyclopentadiene phenol epoxy resin.
4. The adhesive of claim 3, wherein: the molecular formula of the epoxidized hydroxyl-terminated polybutadiene is as follows:
the molecular formula of the dicyclopentadiene phenol epoxy resin is as follows:
5. the adhesive of claim 1, wherein: the filler is silicon dioxide.
6. The adhesive of claim 1, wherein: and the flame retardant further comprises 0-3 parts of an auxiliary agent, wherein the auxiliary agent is one or any combination of a silane coupling agent, a flame retardant, an accelerator and an antioxidant.
7. The adhesive of claim 1, wherein: the solvent is at least one of butanone or cyclohexanone in 10-30 parts.
8. The method for preparing an adhesive according to any one of claims 1 to 7, characterized by comprising the steps of:
step A: sequentially adding polyphenyl ether, filler and solvent into a stirring kettle, mixing and stirring, and then sanding by using a sand mill to prepare a mother solution;
and B: and adding the mother solution, the polyimide solution and the epoxidized polyolefin into a stirring kettle, continuously stirring, stirring for 2-4h, and uniformly mixing to prepare the adhesive.
9. A low dielectric loss pure glue film is characterized in that: the adhesive comprises a release film, an adhesive layer and release paper which are arranged in sequence, wherein the adhesive layer is formed by the adhesive of any one of claims 1-7.
10. The process of claim 9, comprising the steps of: coating an adhesive on a release film, drying the release film coated with the adhesive for 100-500 s at 120-180 ℃ in an oven, and pressing the release film coated with the adhesive surface with release paper at 50-100 ℃ to prepare the low dielectric loss pure adhesive film.
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Application publication date: 20211231 |