CN115851222B - Soft copper foil substrate bonding material and preparation method thereof - Google Patents
Soft copper foil substrate bonding material and preparation method thereof Download PDFInfo
- Publication number
- CN115851222B CN115851222B CN202211433971.6A CN202211433971A CN115851222B CN 115851222 B CN115851222 B CN 115851222B CN 202211433971 A CN202211433971 A CN 202211433971A CN 115851222 B CN115851222 B CN 115851222B
- Authority
- CN
- China
- Prior art keywords
- parts
- epoxy resin
- stirring
- rotating speed
- copper foil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000463 material Substances 0.000 title claims abstract description 39
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000011889 copper foil Substances 0.000 title claims abstract description 22
- 239000000758 substrate Substances 0.000 title claims description 10
- 238000002360 preparation method Methods 0.000 title claims description 6
- 239000003822 epoxy resin Substances 0.000 claims abstract description 47
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 47
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229920002396 Polyurea Polymers 0.000 claims abstract description 23
- 239000012745 toughening agent Substances 0.000 claims abstract description 13
- 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 abstract description 12
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 150000004984 aromatic diamines Chemical class 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 47
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 12
- 150000001412 amines Chemical class 0.000 claims description 12
- 229920000570 polyether Polymers 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000005086 pumping Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229920001721 polyimide Polymers 0.000 abstract description 11
- 230000008901 benefit Effects 0.000 abstract description 9
- 239000004020 conductor Substances 0.000 abstract description 3
- 229920006267 polyester film Polymers 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 17
- 239000004642 Polyimide Substances 0.000 description 9
- 229920000728 polyester Polymers 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 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 description 4
- 241000283690 Bos taurus Species 0.000 description 3
- 125000003700 epoxy group Chemical group 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 229920002799 BoPET Polymers 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 125000001731 2-cyanoethyl group Chemical group [H]C([H])(*)C([H])([H])C#N 0.000 description 1
- KXDHJXZQYSOELW-UHFFFAOYSA-M Carbamate Chemical compound NC([O-])=O KXDHJXZQYSOELW-UHFFFAOYSA-M 0.000 description 1
- HECLRDQVFMWTQS-UHFFFAOYSA-N Dicyclopentadiene Chemical compound C1C2C3CC=CC3C1C=C2 HECLRDQVFMWTQS-UHFFFAOYSA-N 0.000 description 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000001951 carbamoylamino group Chemical group C(N)(=O)N* 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000004148 curcumin Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention relates to a flexible copper foil base material bonding material, which consists of the following raw materials: 30-43 parts of self-synthesized polyurea modified epoxy resin, 25-35 parts of dicyclopentadiene phenol type epoxy resin, 10-20 parts of toughening agent, 10-20 parts of aromatic diamine curing agent and 2-5 parts of imidazole addition compound. The bonding material prepared by the invention has the advantages of convenience in single-component operation, good bonding strength, good toughness, low dielectric constant, good high and low temperature resistance, good wet heat resistance and the like, and is suitable for structural bonding of insulating base film materials such as polyester films or polyimide films in flexible copper foil base materials and copper foil conductor materials.
Description
Technical Field
The invention relates to a soft copper foil substrate bonding material and a preparation method thereof, belonging to the field of adhesives.
Background
The consumer electronics products are rapidly developing towards the light-weight, miniaturized and high-efficiency production directions, and the flexible copper foil substrate (FCCL) has the advantages of light weight, thinness and flexibility, low dielectric constant, good thermal performance, high reliability and the like. Low dielectric constant (Dk) allows for rapid transmission of electrical signals. The thermal performance is good, so that the electronic component is easy to cool. The high reliability allows the electronic assembly to perform well even in severe temperature and humidity environments. In addition, the flexible copper foil base material (FCCL) can be manufactured into a continuous coiled form, and the FCCL is adopted to produce the printed circuit board, so that automatic continuous production can be realized. Flexible copper foil substrates (FCCL) are replacing the key role of Printed Circuit Boards (PCBs) in connecting electronic components in series within advanced consumer electronics.
The flexible copper foil base material (FCCL) is composed of a copper foil conductor, a Polyester (PET) film or a Polyimide (PI) film and an adhesive material, wherein the adhesive material is used for carrying out structural adhesion on the PET film or the PI film in the FCCL and the copper foil, and the FCCL has the advantages of good technological operability, high adhesion strength, good toughness, low dielectric constant, good high and low temperature resistance, good wet heat resistance and capability of effectively improving the functionality and reliability of the FCCL.
Most of the bonding materials have the problems of low bonding strength to PET films or PI films, poor toughness, high dielectric constant, poor reliability and the like, and cannot meet various high-performance requirements of the current flexible copper foil base material (FCCL).
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the bonding material for the soft copper foil base material, and the bonding material prepared by the invention has the advantages of convenience in single-component operation, good bonding strength, good toughness, low dielectric constant, good high-low temperature resistance, good wet heat resistance and the like.
The technical scheme for solving the technical problems is as follows: the preparation method of the flexible copper foil substrate bonding material comprises the following steps:
a. the weight portions are as follows: 79-81 parts of amine-terminated polyether is added into a reaction kettle, heated to 110-120 ℃, set at 20RPM, stirred for 1-2 hours under the condition of vacuumizing, and dehydrated. Cooling to 45-55 ℃, dropwise adding 5-6 parts of toluene diisocyanate, setting the rotating speed to 30RPM, stirring under the protection of nitrogen, finishing dropwise adding within 20-30 minutes, heating to 80-90 ℃, setting the rotating speed to 40RPM under the condition of vacuumizing, and stirring for 1-2 hours; adding 14-15 parts of tetraglycidyl amine type epoxy resin, increasing the temperature to 105-115 ℃, setting the rotating speed to 40RPM under the vacuumizing condition, and stirring for 2-3 hours to prepare the self-synthesized polyurea modified epoxy resin;
b. the weight portions are as follows: 30-43 parts of self-synthesized polyurea modified epoxy resin, 25-35 parts of dicyclopentadiene phenol type epoxy resin, 10-20 parts of toughening agent, 10-20 parts of aromatic diamine curing agent and 2-5 parts of imidazole addition compound are sequentially put into a stirring kettle, and the stirring is carried out for 3-4 hours under the condition of vacuum pumping at a set rotating speed of 30 RPM.
On the basis of the technical scheme, the invention also improves as follows.
Furthermore, the synthesis mechanism of the self-synthesis polyurea modified epoxy resin is that the amine-terminated group of the amine-terminated polyether molecular chain contains active hydrogen and reacts with isocyanate groups of toluene diisocyanate molecular chain to generate ureido (-NHCONH-) and the polarity is stronger than carbamate (-NHCOO-) formed by the reaction of hydroxyl and isocyanate groups under the action of adjacent double hydrogen bonds. The polyurea structure has strong intermolecular force, and shows good toughness, high and low temperature resistance and moist heat resistance. Further, the active hydrogen in the urea group and the epoxy group and the hydroxyl group in the epoxy resin are subjected to addition reaction.
The adoption of the further scheme has the advantages that the epoxy group of the molecular chain end group in the self-synthesized polyurea modified epoxy resin can participate in the next curing and crosslinking, the system compatibility is increased, and the effect of uniform mixing is further achieved; the polyurea structure in the molecular chain has excellent toughness, high and low temperature resistance and damp-heat resistance.
Further, the amine-terminated polyether is CAD2000 manufactured by new material stock, inc.
The amino-terminated polyether has the advantages of high reaction activity, moderate molecular weight and good toughness.
Further, the toluene diisocyanate was TDI-80 manufactured by Wanhua chemical group Co., ltd.
Further, the tetraglycidyl amine type epoxy resin is SW-80 manufactured by Hunan Seivoxine materials science and technology Co.
The adoption of the further scheme has the beneficial effects that the tetraglycidyl amine type epoxy resin has excellent reactivity, bonding strength and heat resistance, and a plurality of epoxy groups on a molecular structure are beneficial to the further reactivity of the polyurea modified epoxy resin synthesized with the polyurea groups.
Further, the dicyclopentadiene phenol type epoxy resin is HQCE-11 produced by Hunan Seivesnew materials science and technology Co., ltd, and the specific structural formula is shown as formula 1:
1 (1)
The dicyclopentadiene phenol type epoxy resin has a DCPD type structure with a special framework, and has the characteristics of excellent wet heat resistance, low dielectric constant and high bonding strength.
Further, the toughening agent is XT100 manufactured by ARKEMA, france.
The adoption of the further scheme has the beneficial effects that the toughening agent is uniformly dispersed in the epoxy resin by the nano rubber particles, has excellent compatibility, stability and toughness, and does not reduce the heat resistance of the product.
Further, the aromatic diamine curing agent is E100 produced by Zhangjia Kong elegance chemical industry Co., ltd, and the specific structural formula is shown as formula 2:
2, 2
The aromatic diamine has the advantages of good room temperature storage stability, high bonding strength, low curing shrinkage and good moist heat resistance.
Further, the imidazole adduct is 2E4MZ-CN manufactured by Kagaku Kogyo Co., ltd., the specific structural formula of which is shown in formula 3:
3
The imidazole adduct has cyanoethyl functional groups, and has the characteristics of product curing promotion, high bonding strength and good wet heat resistance.
The beneficial effects of the invention are as follows: the bonding material has the advantage of good bonding strength, and is suitable for bonding structures of various polyester film or polyimide film substrates and copper foil substrates. The high toughness effectively meets the requirement that the soft copper foil base material (FCCL) is made into a continuous coiled form without degumming and cracking. The low dielectric constant effectively ensures the requirement of rapid transmission of the electric signal. The FCCL has good high and low temperature resistance and good moisture and heat resistance, and the prepared FCCL has good functionality and applicability.
Detailed Description
The principles and features of the present invention are described below with examples given for the purpose of illustration only and are not intended to limit the scope of the invention.
Example 1
a. The weight portions are as follows: adding 2000 800g of amine-terminated polyether CAD into a reaction kettle, heating to 110 ℃, setting the rotating speed to 20RPM, stirring for 1.5 hours under the condition of vacuumizing, and dehydrating. Cooling to 55 ℃, dropwise adding 50g of toluene diisocyanate TDI-80 g, setting the rotating speed to 30RPM, stirring under the protection of nitrogen, finishing dropwise adding within 30 minutes, heating to 80 ℃, setting the rotating speed to 40RPM under the condition of vacuumizing, and stirring for 1 hour; adding tetraglycidyl amine type epoxy resin SW-80 150g, increasing the temperature to 105 ℃, setting the rotating speed to 40RPM under the vacuumizing condition, and stirring for 2.5 hours to prepare the self-synthesized polyurea modified epoxy resin;
b. the weight portions are as follows: 300g of self-synthesized polyurea modified epoxy resin, 300g of dicyclopentadiene phenol type epoxy resin HQCE-11 g, 100g of toughening agent XT-100 g, 100 200g of aromatic diamine curing agent E and 50g of imidazole adduct 2E4MZ-CN are sequentially put into a stirring kettle, and the stirring is carried out for 3.5 hours under the condition of vacuum pumping at the set rotating speed of 30RPM, so as to obtain the bonding material.
Example 2
a. The weight portions are as follows: adding 2000 800g of amine-terminated polyether CAD into a reaction kettle, heating to 110 ℃, setting the rotating speed to 20RPM, stirring for 1.5 hours under the condition of vacuumizing, and dehydrating. Cooling to 55 ℃, dropwise adding 50g of toluene diisocyanate TDI-80 g, setting the rotating speed to 30RPM, stirring under the protection of nitrogen, finishing dropwise adding within 30 minutes, heating to 85 ℃, setting the rotating speed to 40RPM under the condition of vacuumizing, and stirring for 2 hours; adding tetraglycidyl amine type epoxy resin SW-80 150g, increasing the temperature to 105 ℃, setting the rotating speed to 40RPM under the vacuumizing condition, and stirring for 2.5 hours to prepare the self-synthesized polyurea modified epoxy resin;
b. the weight portions are as follows: 350g of self-synthesized polyurea modified epoxy resin, 300g of dicyclopentadiene phenol type epoxy resin HQCE-11, 160g of toughening agent XT-100, 100 150g of aromatic diamine curing agent E and 40g of imidazole adduct 2E4MZ-CN are sequentially put into a stirring kettle, and the stirring is carried out for 3.5 hours under the condition of vacuum pumping at the set rotating speed of 30RPM, so as to obtain the bonding material.
Example 3
a. The weight portions are as follows: adding 2000 800g of amine-terminated polyether CAD into a reaction kettle, heating to 120 ℃, setting the rotating speed to 20RPM, stirring for 1 hour under the condition of vacuumizing, and dehydrating. Cooling to 55 ℃, dropwise adding 50g of toluene diisocyanate TDI-80 g, setting the rotating speed to 30RPM, stirring under the protection of nitrogen, finishing dropwise adding within 30 minutes, heating to 85 ℃, setting the rotating speed to 40RPM under the condition of vacuumizing, and stirring for 2 hours; adding tetraglycidyl amine type epoxy resin SW-80 150g, increasing the temperature to 105 ℃, setting the rotating speed to 40RPM under the vacuumizing condition, and stirring for 2.5 hours to prepare the self-synthesized polyurea modified epoxy resin;
b. the weight portions are as follows: 430g of self-synthesized polyurea modified epoxy resin, 250g of dicyclopentadiene phenol type epoxy resin HQCE-11 g, 200g of toughening agent XT-100 g, 100 100g of aromatic diamine curing agent E and 20g of imidazole adduct 2E4MZ-CN are sequentially put into a stirring kettle, and the stirring is carried out for 3.5 hours under the condition of vacuum pumping at the set rotating speed of 30RPM, so as to obtain the bonding material.
Comparative example 1
a. The weight portions are as follows: adding 2000 650g of amine-terminated polyether CAD into a reaction kettle, heating to 110 ℃, setting the rotating speed to 20RPM, stirring for 1.5 hours under the condition of vacuumizing, and dehydrating. Cooling to 55 ℃, dropwise adding toluene diisocyanate TDI-80 150g, setting the rotating speed to 30RPM, stirring under nitrogen protection, finishing dropwise adding within 2 hours, heating to 80 ℃, setting the rotating speed to 40RPM under vacuum pumping, and stirring for 2 hours; adding 200g of tetraglycidyl amine type epoxy resin SW-80 g, increasing the temperature to 105 ℃, setting the rotating speed to 40RPM under the vacuumizing condition, and stirring for 2.5 hours to prepare the self-synthesis polyurea modified epoxy resin;
b. the weight portions are as follows: 300g of self-synthesized polyurea modified epoxy resin, 300g of dicyclopentadiene phenol type epoxy resin HQCE-11 g, 100g of toughening agent XT-100 g, 100 200g of aromatic diamine curing agent E and 50g of imidazole adduct 2E4MZ-CN are sequentially put into a stirring kettle, and the stirring is carried out for 3.5 hours under the condition of vacuum pumping at the set rotating speed of 30RPM, so as to obtain the bonding material.
Comparative example 2
The weight portions are as follows: 150g of bisphenol A type epoxy resin E, 11 g of dicyclopentadiene phenol type epoxy resin HQCE-11 g, 100g of toughening agent XT-100 g, 100 250g of aromatic diamine curing agent E and 50g of imidazole adduct 2E4MZ-CN are sequentially put into a stirring kettle, the rotating speed is set to 30RPM under the vacuumizing condition, and the stirring is carried out for 3.5 hours, thus obtaining the bonding material.
Comparative example 3
a. The weight portions are as follows: adding 2000 800g of amine-terminated polyether CAD into a reaction kettle, heating to 110 ℃, setting the rotating speed to 20RPM, stirring for 1.5 hours under the condition of vacuumizing, and dehydrating. Cooling to 55 ℃, dropwise adding 50g of toluene diisocyanate TDI-80 g, setting the rotating speed to 30RPM, stirring under the protection of nitrogen, finishing dropwise adding within 30 minutes, heating to 85 ℃, setting the rotating speed to 40RPM under the condition of vacuumizing, and stirring for 2 hours; adding tetraglycidyl amine type epoxy resin SW-80 150g, increasing the temperature to 105 ℃, setting the rotating speed to 40RPM under the vacuumizing condition, and stirring for 2.5 hours to prepare the self-synthesized polyurea modified epoxy resin;
b. the weight portions are as follows: 350g of self-synthesized polyurea modified epoxy resin, 290g of bisphenol A type epoxy resin E51 g, 160g of toughening agent XT-100 g, 100 160g of aromatic diamine curing agent E and 40g of imidazole adduct 2E4MZ-CN are sequentially put into a stirring kettle, and the stirring kettle is stirred for 3.5 hours under the condition of vacuum pumping at the set rotating speed of 30 RPM.
Comparative example 4
a. The weight portions are as follows: adding 2000 800g of amine-terminated polyether CAD into a reaction kettle, heating to 110 ℃, setting the rotating speed to 20RPM, stirring for 1.5 hours under the condition of vacuumizing, and dehydrating. Cooling to 55 ℃, dropwise adding 50g of toluene diisocyanate TDI-80 g, setting the rotating speed to 30RPM, stirring under the protection of nitrogen, finishing dropwise adding within 30 minutes, heating to 85 ℃, setting the rotating speed to 40RPM under the condition of vacuumizing, and stirring for 2 hours; adding tetraglycidyl amine type epoxy resin SW-80 150g, increasing the temperature to 105 ℃, setting the rotating speed to 40RPM under the vacuumizing condition, and stirring for 2.5 hours to prepare the self-synthesized polyurea modified epoxy resin;
b. the weight portions are as follows: 350g of self-synthesized polyurea modified epoxy resin, 300g of dicyclopentadiene phenol type epoxy resin HQCE-11, 160g of toughening agent XT-100, 150g of aliphatic modified amine curing agent MY-24 and 40g of imidazole adduct 2E4MZ-CN are sequentially put into a stirring kettle, and the stirring is carried out for 3.5 hours under the condition of vacuum pumping at the set rotating speed of 30RPM, so as to obtain the bonding material.
Specific test examples
The performance of the structural adhesives of the present invention of examples 1-3 and comparative examples 1-4 above was tested by the following test. Wherein, the bonding strength performance is characterized by the stripping force of a Polyester (PET) film or a Polyimide (PI) film to the copper foil, and the larger the numerical value is, the better the bonding strength performance is characterized; the toughness performance is characterized by tensile strength and elongation at break, and the larger the numerical value is, the better the toughness performance is characterized; the low dielectric constant performance is characterized by a dielectric constant value, and the smaller the value is, the better the performance is characterized; the high-low temperature resistance is characterized by the stripping force after aging of a high-low temperature cold-hot impact box, and the larger the numerical value is, the better the performance is characterized; the wet heat resistance is characterized by the stripping force after aging in a high-temperature high-humidity environment box, and the larger the numerical value is, the better the performance is.
Test example 1 adhesive Strength Performance test
And using a universal tester, selecting PET and PI Vs copper foil materials, and testing the stripping force in cattle (N) according to the pressure-sensitive adhesive tape stripping force test method, the temperature is 25 ℃, the displacement control rate is 10 mm/min.
Test example 2 toughness test
Preparing a dumbbell-shaped sample sheet from the bonding material by using a universal testing machine, and testing tensile strength in megapascals (MPa) according to a test method of tensile stress strain property of thermoplastic rubber at 25 ℃ and a displacement control rate of 10 mm/min; elongation at break, percent (%).
Test example 3 Low dielectric constant Performance test
The relative permittivity value was measured in 1 using a permittivity tester with an output voltage of 200V and a frequency range of 50 HZ.
Test example 4 high and Low temperature resistance test
The peeling force was measured in bovine (N) by the method of test example 1 after 500 cycles at-40 to 125℃using a high and low temperature cold and hot shock box.
Test example 5 moisture and thermal resistance test
The peeling force was measured in bovine (N) by the method of test example 1 after 500 hours with the use of a high temperature and high humidity environmental chamber at a set condition temperature of 85℃and humidity of 85%.
The test results are shown in table 1 below.
TABLE 1 test results for samples prepared in examples 1-3 and comparative examples 1-4
As can be seen from the data in Table 1, the bonding material prepared by the invention has the advantages of convenient single-component operation, good bonding strength, good toughness, low dielectric constant, good high and low temperature resistance, good wet heat resistance and the like, and is suitable for structural bonding of insulating base film materials such as Polyester (PET) films or Polyimide (PI) films and copper foil conductor materials in flexible copper foil substrates (FCCL).
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (4)
1. The preparation method of the flexible copper foil substrate bonding material is characterized by comprising the following steps of: a. the weight portions are as follows: 79-81 parts of amine-terminated polyether is added into a reaction kettle, heated to 110-120 ℃, set for 20RPM, stirred for 1-2 hours under the condition of vacuum pumping, and dehydrated; cooling to 45-55 ℃, dropwise adding 5-6 parts of toluene diisocyanate, setting the rotating speed to 30RPM, stirring under the protection of nitrogen, finishing dropwise adding within 20-30 minutes, heating to 80-90 ℃, setting the rotating speed to 40RPM under the condition of vacuumizing, and stirring for 1-2 hours; adding 14-15 parts of tetraglycidyl amine type epoxy resin, increasing the temperature to 105-115 ℃, setting the rotating speed to 40RPM under the vacuumizing condition, and stirring for 2-3 hours to prepare the self-synthesized polyurea modified epoxy resin;
b. the weight portions are as follows: 30-43 parts of self-synthesized polyurea modified epoxy resin, 25-35 parts of dicyclopentadiene phenol type epoxy resin, 10-20 parts of toughening agent, 10-20 parts of aromatic diamine curing agent and 2-5 parts of imidazole addition compound are sequentially put into a stirring kettle, and are stirred for 3-4 hours under the condition of vacuum pumping at a set rotating speed of 30 RPM;
the aromatic diamine curing agent is produced by Zhangjia Kong Yarui chemical Co., ltdE100 of (2), the specific structural formula is:。
2. the method of claim 1, wherein the amine-terminated polyether is CAD2000 manufactured by new material stock, inc. In morning; the toluene diisocyanate is TDI-80 produced by Wanhua chemical group Co., ltd; the tetraglycidyl amine type epoxy resin is SW-80 produced by Hunan Seivoxine materials science and technology Co.
3. The preparation method according to claim 1, wherein the dicyclopentadiene phenol type epoxy resin is HQCE-11 manufactured by hunan sai er weixin materials science co.
4. The method of manufacture of claim 1, wherein the toughening agent is XT100 produced by ARKEMA, france; the imidazole adduct is 2E4MZ-CN manufactured by Kagaku Kogyo Co., ltd.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211433971.6A CN115851222B (en) | 2022-11-16 | 2022-11-16 | Soft copper foil substrate bonding material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211433971.6A CN115851222B (en) | 2022-11-16 | 2022-11-16 | Soft copper foil substrate bonding material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115851222A CN115851222A (en) | 2023-03-28 |
| CN115851222B true CN115851222B (en) | 2024-04-02 |
Family
ID=85663717
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211433971.6A Active CN115851222B (en) | 2022-11-16 | 2022-11-16 | Soft copper foil substrate bonding material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115851222B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1143661A (en) * | 1996-01-17 | 1997-02-26 | 青岛化工学院 | Process for preparing normal temp solidification polyurethane toughened epoxy resin adhesive |
| JP2001031739A (en) * | 1999-07-22 | 2001-02-06 | Nippon Paint Co Ltd | Aminopolyether-modified epoxy and cationic electrodepostion coating composition containing the same |
| TW200403298A (en) * | 2002-07-01 | 2004-03-01 | Vantico Ag | Isocyanato-containing polyether urethane monoepoxides |
| CN101880372A (en) * | 2010-06-25 | 2010-11-10 | 广东新劲刚超硬材料有限公司 | Active prepolymer, preparation method thereof and polyurea adhesive and epoxy resin adhesive containing the same |
| CN102311715A (en) * | 2010-07-09 | 2012-01-11 | 上海海鹰粘接科技有限公司 | Healant for chemical pipes and preparation method thereof |
| CN106632971A (en) * | 2016-12-19 | 2017-05-10 | 钦州市高新技术产业服务中心 | Anticorrosive material for epoxy resin and preparation method of anticorrosive material |
-
2022
- 2022-11-16 CN CN202211433971.6A patent/CN115851222B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1143661A (en) * | 1996-01-17 | 1997-02-26 | 青岛化工学院 | Process for preparing normal temp solidification polyurethane toughened epoxy resin adhesive |
| JP2001031739A (en) * | 1999-07-22 | 2001-02-06 | Nippon Paint Co Ltd | Aminopolyether-modified epoxy and cationic electrodepostion coating composition containing the same |
| TW200403298A (en) * | 2002-07-01 | 2004-03-01 | Vantico Ag | Isocyanato-containing polyether urethane monoepoxides |
| CN101880372A (en) * | 2010-06-25 | 2010-11-10 | 广东新劲刚超硬材料有限公司 | Active prepolymer, preparation method thereof and polyurea adhesive and epoxy resin adhesive containing the same |
| CN102311715A (en) * | 2010-07-09 | 2012-01-11 | 上海海鹰粘接科技有限公司 | Healant for chemical pipes and preparation method thereof |
| CN106632971A (en) * | 2016-12-19 | 2017-05-10 | 钦州市高新技术产业服务中心 | Anticorrosive material for epoxy resin and preparation method of anticorrosive material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115851222A (en) | 2023-03-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5015591B2 (en) | Epoxy resin composition | |
| CN100441652C (en) | Method for preparing binder of polyimide of containing phenolic hydroxyl group | |
| CN109957203B (en) | Resin composition, prepreg, and copper foil substrate | |
| CN113004856B (en) | high-Tg thermosetting resin composition and preparation method and application thereof | |
| KR101749369B1 (en) | Composition for film, and adhesive film and cover lay film formed therefrom | |
| CN109504033A (en) | A kind of flexibility prepreg and preparation method thereof | |
| CN115777003A (en) | Isocyanate-modified polyimide resin, resin composition, and cured product thereof | |
| CN115851222B (en) | Soft copper foil substrate bonding material and preparation method thereof | |
| CN114148048A (en) | High-heat-dissipation aluminum-based copper-clad plate and preparation method thereof | |
| CN115806665A (en) | Bismaleimide-modified polyphenylene ether resin, method for producing same, and substrate material | |
| CN116120560B (en) | Preparation method of modified bismaleimide prepolymer, resin composition and application of resin composition | |
| CN115073693A (en) | Toughening resin-based conductive silver paste and preparation method thereof | |
| US5326794A (en) | Barbituric acid-modified bismaleimide with diamine and polyisocyanate-modified epoxy resin | |
| JP4172179B2 (en) | Thermosetting resin composition, adhesive film, copper-clad laminate and printed wiring board | |
| CN114974651A (en) | Epoxy resin-based conductive slurry and preparation method and application thereof | |
| KR20170025304A (en) | Resin composition for EMI shielding film and EMI shielding film using the same | |
| CN114589991A (en) | Method for preparing high-speed copper-clad plate by using bismaleimide modified hydrocarbon resin | |
| CN109705387B (en) | Halogen-free resin composition, cover film for flexible printed circuit board containing same and flexible printed circuit board | |
| CN117384354B (en) | Resin composition for copper-clad plate and application thereof | |
| CN111944274A (en) | Bendable prepreg gumming solution for circuit board, prepreg and preparation method of prepreg | |
| CN109266297A (en) | A kind of high-temperature Resistance Adhesives and its preparation method and application | |
| CN112877006B (en) | Hot-pressing insulating film and flexible flat cable comprising same | |
| CN115109387B (en) | Resin composition and application thereof | |
| CN110628310A (en) | Multilayer structure and substrate | |
| KR102094918B1 (en) | diamine compound, polyiamic acid resin composition containing the same, polyimide resin containing the same, adhesive for flexible circuit clad layer containing the same and manufacturing method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |