CN115678488A - High-temperature-resistant adhesive and flexible copper clad laminate prepared from same - Google Patents
High-temperature-resistant adhesive and flexible copper clad laminate prepared from same Download PDFInfo
- Publication number
- CN115678488A CN115678488A CN202211096062.8A CN202211096062A CN115678488A CN 115678488 A CN115678488 A CN 115678488A CN 202211096062 A CN202211096062 A CN 202211096062A CN 115678488 A CN115678488 A CN 115678488A
- Authority
- CN
- China
- Prior art keywords
- polyimide
- adhesive
- temperature resistant
- solution
- paa
- 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.)
- Pending
Links
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 141
- 239000000853 adhesive Substances 0.000 title claims abstract description 137
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 62
- 239000010949 copper Substances 0.000 title claims abstract description 62
- 229920001721 polyimide Polymers 0.000 claims abstract description 162
- 239000004642 Polyimide Substances 0.000 claims abstract description 132
- 238000003756 stirring Methods 0.000 claims abstract description 64
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000003822 epoxy resin Substances 0.000 claims abstract description 39
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 39
- 239000003063 flame retardant Substances 0.000 claims abstract description 31
- 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 abstract description 30
- 239000009719 polyimide resin Substances 0.000 claims abstract description 29
- 239000007787 solid Substances 0.000 claims abstract description 24
- 238000000576 coating method Methods 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 239000011248 coating agent Substances 0.000 claims abstract description 18
- 230000009477 glass transition Effects 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims description 47
- 238000005303 weighing Methods 0.000 claims description 26
- 238000002360 preparation method Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 19
- 239000000843 powder Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 13
- 239000011889 copper foil Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000004132 cross linking Methods 0.000 claims description 3
- 238000007731 hot pressing Methods 0.000 claims description 3
- 239000002648 laminated material Substances 0.000 claims description 3
- 238000003475 lamination Methods 0.000 claims description 3
- 229940113088 dimethylacetamide Drugs 0.000 claims 7
- 230000005012 migration Effects 0.000 abstract description 3
- 238000013508 migration Methods 0.000 abstract description 3
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 10
- 239000003292 glue Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 229920006332 epoxy adhesive Polymers 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 229920002312 polyamide-imide Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920000459 Nitrile rubber Polymers 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000004962 Polyamide-imide Substances 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000013538 functional additive Substances 0.000 description 1
- 150000003949 imides Chemical group 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
Landscapes
- Laminated Bodies (AREA)
Abstract
The invention discloses a high temperature resistant adhesive and a flexible copper clad laminate made of the same, wherein a Polyimide (PAA) adhesive solution with the solid content of 22% is prepared by stirring, dissolving, stirring and mixing polyimide resin, JER-1256 ultrahigh molecular weight epoxy resin, OP-935 flame retardant and DMAC dimethylacetamide according to the weight ratio; then coating a Polyimide (PAA) adhesive solution on a Polyimide (PI) film to prepare a non-adhesive flexible copper clad laminate with a high Tg (glass transition temperature) point, wherein the non-adhesive flexible copper clad laminate has excellent heat resistance, adhesive property, flame retardance, ion migration resistance and weather resistance; can be suitable for the high heat-resistant field of high-end circuit boards.
Description
Technical Field
The invention relates to a high-temperature-resistant adhesive and a flexible copper clad laminate prepared from the same. In particular to a flexible copper clad laminate prepared by preparing a high temperature resistant adhesive and coating the adhesive on a copper foil.
Background
A class of polymers containing an imide structure in the main chain is called polyimide, which has extremely strong temperature resistance, extremely high strength and modulus, low linear expansion coefficient, good chemical corrosion resistance and the like, and the excellent properties make the polyimide have various uses; the good high temperature resistance enables the polyimide to occupy an important position in the field of temperature-resistant adhesives, but when only one material of the polyimide is used as the adhesive, the polyimide adhesive has a plurality of defects, and the application fields of the polyimide adhesive are limited, such as more complex curing process, high curing temperature, larger colloid shrinkage and poorer adhesive property.
The Flexible Copper Clad Laminate (FCCL) mainly refers to a copper clad laminate with good flexibility and manufactured by taking high-temperature resistant Polyimide (PI) as an insulation base film, and compared with the traditional rigid copper clad laminate, the flexible copper clad laminate has the characteristics of light weight, thinness, small volume, flexibility and capability of three-dimensional wiring, thereby being widely favored; the flexible printed circuit board manufactured by the flexible copper clad laminate is widely applied to portable electronic equipment such as mobile phones, digital cameras, digital video cameras and notebook computers, and the fields of flat televisions, office automation equipment, automotive electronics, instruments and meters, medical machinery, aerospace and war industry; the FCCL market will show a clear upward trend thanks to the rapid development of emerging markets such as smart electronics.
The flexible copper clad laminate mainly comprises glue products, wherein the products comprise three layers of materials, namely copper foil, polyimide film and adhesive; the products are also called three-layer flexible copper clad laminates, the adhesives used by the three-layer flexible copper clad laminates are mostly epoxy adhesives and acrylate adhesives, and the two adhesives have limited heat resistance; with the rapid development of the electronic industry, electronic products are further miniaturized, lightened and assembled and densified, and three-layer flexible copper clad laminates cannot meet the use requirements in the aspects of heat resistance, chemical resistance, flame retardance, dimensional stability and long-term reliability, so that the flexible copper clad laminates gradually develop to glue-free products; the flexible copper clad laminate without glue is different from the flexible copper clad laminate with glue in that epoxy adhesive and acrylate adhesive are not used, the flexible copper clad laminate without glue is also called a two-layer flexible copper clad laminate, namely conductive layer copper and insulating layer polyimide, and the two-layer flexible copper clad laminate has higher heat resistance, higher dimensional stability, more excellent flexibility and more excellent long-term reliability.
The non-adhesive flexible copper clad laminate has very high heat-resisting requirement, and the current two-layer flexible copper clad laminate mainly has three methods to realize the non-adhesive double-sided board, namely, a polyamide imide PAI coating method, which has the defects of low peeling strength and fragile adhesive layer which is not beneficial to pressing the copper foil; secondly, the thermoplastic TPI high-temperature compression method has the defects that the equipment investment cost is high, raw materials are not easy to obtain, and the equipment and the raw materials are imported abroad; the sputtering method has the disadvantages of large equipment investment, relatively slow production efficiency and incapability of producing thick copper products.
The existing flexible copper clad laminate mainly uses epoxy resin and nitrile rubber as flexible adhesives, but rubber is used for improving the flexibility of the copper clad laminate and playing a role in flexibility, but the TG point of the rubber is very low, and the heat resistance is poor.
Disclosure of Invention
The invention aims to provide a high-temperature-resistant adhesive and a flexible copper clad laminate prepared from the same, which have the advantages of good adhesive property, heat resistance, ion migration resistance and flame retardance, low cost and capability of realizing batch production.
In order to realize the purpose, the high temperature resistant adhesive and the flexible copper clad laminate prepared by the high temperature resistant adhesive are prepared by stirring, dissolving and mixing Polyimide (PAA) adhesive solution with the solid content of 22 percent according to the weight proportion of polyimide resin, JER-1256 ultrahigh molecular weight epoxy resin, OP-935 flame retardant and DMAC dimethylacetamide; then coating a Polyimide (PAA) adhesive solution on the surface of a Polyimide (PI) film, semi-curing and pressing the Polyimide (PAA) adhesive solution on a copper foil to prepare the adhesive-free flexible copper clad laminate with a high Tg (glass transition temperature) point.
A Polyimide (PAA) adhesive was prepared from the following components: (the amount is weight portion)
16-24 parts of polyimide resin, 0.8-1.2 parts of JER-1256 ultrahigh molecular weight epoxy resin, 2.4-3.6 parts of OP-935 flame retardant and 54.4-81.3 parts of DMAC dimethylacetamide.
The preferable weight (part) proportioning range of the formula for preparing the Polyimide (PAA) adhesive is as follows:
19-21 parts of polyimide resin, 0.9-1.1 part of JER-1256 ultrahigh molecular weight epoxy resin, 2.8-3.2 parts of OP-935 flame retardant and 64.4-71.3 parts of DMAC dimethylacetamide.
The optimal weight (part) ratio for preparing the Polyimide (PAA) adhesive is as follows:
polyimide resin 20, JER-1256 ultra-high molecular weight epoxy resin 1, OP-935 flame retardant 3 and DMAC dimethylacetamide 68.
The method for preparing the Polyimide (PAA) adhesive from the components in proportion comprises the following steps:
(1) Preparation of polyimide solution
Respectively weighing the polyimide resin powder 16-24 and the DMAC (dimethylacetamide) 54.4-81.3 in parts by weight, putting the weighed materials into a stirring tank, and stirring the materials at a high speed for 120 minutes to prepare a polyimide solution;
(2) Preparation of high temperature resistant adhesive
Respectively weighing 0.8-1.2 parts of JER-1256 ultrahigh molecular weight epoxy resin and 2.4-3.6 parts of OP-935 flame retardant, placing the materials into a stirring tank, stirring the materials at a high speed for 120 minutes, and fully mixing the materials with polyimide solution to prepare the high temperature resistant Polyimide (PAA) adhesive solution with the solid content of 22 percent.
The method for preparing the adhesive-free flexible copper clad laminate by using the prepared high temperature resistant Polyimide (PAA) adhesive comprises the following steps:
(1) Coating of
The prepared high-temperature resistant Polyimide (PAA) adhesive solution is placed and coated on a Polyimide (PI) film, and the thickness of the coated dry adhesive is controlled to be 5-15 mu m;
(2) Drying the mixture
Putting the coated material into an oven for drying and realizing partial crosslinking, wherein the drying temperature is 160 ℃, and the drying time is 3 minutes;
(3) Pressing together
Placing the dried material on the rough surface of the copper foil, then placing the materials into a coating machine together, and carrying out hot-pressing lamination under the conditions of 160 ℃ and 0.4KGF/cm < 2 > pressure to ensure that the dried material and the rough surface of the copper foil are linearly laminated;
(4) Curing
And (3) placing the laminated material into an oven, and curing for 180 minutes at 180 ℃ to obtain the adhesive-free flexible copper-clad plate with a high Tg (glass transition temperature) point.
In one preferable technical scheme, a multifunctional epoxy resin EPM-420, a 4,4' -DDS epoxy resin curing agent and a 2E4MZ accelerator are added on a base material of the formula of the invention, so that the high-temperature performance and the bonding strength of the adhesive are ensured.
Compared with the prior art, the high-temperature-resistant adhesive and the flexible copper clad laminate prepared by the high-temperature-resistant adhesive have the following excellent effects.
The high temperature resistant adhesive and the flexible copper clad laminate prepared by the high temperature resistant adhesive take self-made soluble polyimide resin powder as main resin, and are matched with epoxy resin and functional additives to prepare the high temperature resistant adhesive, the glass transition temperature of the adhesive can reach 180 ℃, and the heat resistance of the flexible copper clad laminate prepared by the adhesive can reach the level of the flexible copper clad laminate without adhesive; the soluble polyimide adhesive can be used for preparing a glue-free flexible copper clad laminate by a coating method, so that the equipment and raw material cost is greatly reduced, and the prepared glue-free flexible copper clad laminate has excellent heat resistance, adhesive property, flame retardant property, ion migration resistance and weather resistance; the coating method can be suitable for the high-heat-resistance field of high-end circuit boards, and the coating method can gradually replace a high-temperature pressing method in the aspect of the manufacturing process of a two-layer flexible copper-clad plate so as to reduce the production cost.
Multifunctional epoxy resin EPM-420, 4' -DDS epoxy resin curing agent and 2E4MZ accelerator are added to ensure the high-temperature performance and the bonding strength of the adhesive; the silane coupling agent is added to improve the bonding strength, and the phosphorus flame retardant is added to improve the flame retardant property and ensure the adhesive density; and the JER-1256 ultra-high molecular weight epoxy resin is added to meet the requirements of flexibility and bending resistance of the flexible copper clad laminate.
Detailed Description
The high temperature resistant adhesive and the flexible copper clad laminate made therefrom of the invention will be further explained in detail.
The high-temperature-resistant adhesive and the flexible copper clad laminate prepared by the high-temperature-resistant adhesive are prepared by stirring, dissolving and mixing Polyimide (PAA) adhesive solution with the solid content of 22% according to the weight ratio of polyimide resin, JER-1256 ultrahigh molecular weight epoxy resin, OP-935 flame retardant and DMAC dimethylacetamide; then coating a Polyimide (PAA) adhesive solution on a Polyimide (PI) film to prepare the adhesive-free flexible copper clad laminate with a high Tg (glass transition temperature) point.
A Polyimide (PAA) adhesive was prepared from the following components: (amounts are in parts by weight)
16-24 parts of polyimide resin, 0.8-1.2 parts of JER-1256 ultrahigh molecular weight epoxy resin, 2.4-3.6 parts of OP-935 flame retardant and 54.4-81.3 parts of DMAC dimethylacetamide.
The preferable weight (part) proportioning range of the formula for preparing the Polyimide (PAA) adhesive is as follows:
19-21 parts of polyimide resin, 0.9-1.1 part of JER-1256 ultrahigh molecular weight epoxy resin, 2.8-3.2 parts of OP-935 flame retardant and 64.4-71.3 parts of DMAC dimethylacetamide.
The optimal weight (part) ratio for preparing the Polyimide (PAA) adhesive is as follows:
polyimide resin 20, JER-1256 ultra-high molecular weight epoxy resin 1, OP-935 flame retardant 3 and DMAC dimethylacetamide 68.
The method for preparing the Polyimide (PAA) adhesive from the components in proportion comprises the following steps:
(1) Preparation of polyimide solution
Respectively weighing the polyimide resin powder 16-24 and the DMAC (dimethylacetamide) 54.4-81.3 in parts by weight, putting the weighed materials into a stirring tank, and stirring the materials at a high speed for 120 minutes to prepare a polyimide solution;
(2) Preparation of high temperature resistant adhesive
Respectively weighing 0.8-1.2 parts by weight of JER-1256 ultra-high molecular weight epoxy resin and 2.4-3.6 parts by weight of OP-935 flame retardant, placing into a stirring tank, stirring at high speed for 120 minutes, and fully mixing with polyimide solution to prepare the high temperature resistant Polyimide (PAA) adhesive solution with the solid content of 22%.
The method for manufacturing the non-adhesive flexible copper clad laminate by using the prepared high temperature resistant Polyimide (PAA) adhesive comprises the following steps:
(1) Coating of
Placing and coating the prepared high-temperature-resistant Polyimide (PAA) adhesive solution on a Polyimide (PI) film, wherein the thickness of the coated dry adhesive is controlled to be 5-15 mu m;
(2) Drying by baking
Putting the coated material into an oven for drying and realizing partial crosslinking, wherein the drying temperature is 160 ℃, and the drying time is 3 minutes;
(3) Pressing together
Placing the dried material on the rough surface of the copper foil, then placing the materials into a coating machine together, and carrying out hot-pressing lamination under the conditions of 160 ℃ and 0.4KGF/cm < 2 > pressure to ensure that the dried material and the rough surface of the copper foil are linearly laminated;
(4) Curing of
And (3) placing the laminated material into an oven, and curing for 180 minutes at 180 ℃ to obtain the adhesive-free flexible copper-clad plate with a high Tg (glass transition temperature) point.
When the high-temperature-resistant adhesive is prepared, a multifunctional epoxy resin EPM-420, a 4,4' -DDS epoxy resin curing agent and a 2E4MZ accelerator are added, and the mixture is continuously stirred for 120 to 360 minutes to prepare a Polyimide (PAA) adhesive solution with the solid content of 22 percent, so that the high-temperature performance and the bonding strength of the adhesive are ensured.
Example 1
The high-temperature-resistant adhesive and the flexible copper clad laminate prepared by the high-temperature-resistant adhesive are prepared by stirring, dissolving and mixing Polyimide (PAA) adhesive solution with the solid content of 22% according to the weight ratio of polyimide resin, JER-1256 ultrahigh molecular weight epoxy resin, OP-935 flame retardant and DMAC dimethylacetamide; then coating a Polyimide (PAA) adhesive solution on a Polyimide (PI) film to prepare the adhesive-free flexible copper clad laminate with a high Tg (glass transition temperature) point.
The method for preparing the high-temperature resistant Polyimide (PAA) adhesive from the components in proportion comprises the following steps:
(1) Preparing polyimide solution
Respectively weighing the polyimide resin powder 24 and the DMAC dimethylacetamide 54.4 according to the weight ratio, putting the materials into a stirring tank together, and stirring the materials at a high speed for 120 minutes to prepare a polyimide solution;
(2) Preparation of high temperature resistant adhesive
Respectively weighing the components according to the weight ratio of JER-1256 ultra-high molecular weight epoxy resin 1.2 to OP-935 flame retardant 2.4, placing the components into a stirring tank, stirring the components at a high speed for 120 minutes, and fully mixing the components with a polyimide solution to prepare a high temperature resistant Polyimide (PAA) adhesive solution with the solid content of 22 percent.
Example 2
The high temperature resistant adhesive and the flexible copper clad laminate prepared by the high temperature resistant adhesive are prepared by stirring, dissolving and mixing Polyimide (PAA) adhesive solution with the solid content of 22 percent according to the weight proportion of polyimide resin, JER-1256 ultrahigh molecular weight epoxy resin, OP-935 flame retardant and DMAC dimethylacetamide; then coating a Polyimide (PAA) adhesive solution on a Polyimide (PI) film to prepare the adhesive-free flexible copper clad laminate with a high Tg (glass transition temperature) point.
The method for preparing the high-temperature resistant Polyimide (PAA) adhesive from the components in proportion is as follows:
(1) Preparing polyimide solution
Respectively weighing the polyimide resin powder 16 and the DMAC dimethylacetamide 81.3 according to the weight ratio, putting the materials into a stirring tank together, and stirring the materials at a high speed for 120 minutes to prepare a polyimide solution;
(2) Preparation of high temperature resistant adhesive
Respectively weighing 0.8 parts of JER-1256 ultrahigh molecular weight epoxy resin and 3.6 parts of OP-935 flame retardant, placing into a stirring tank, stirring at high speed for 120 minutes, and fully mixing with the polyimide solution to prepare the high temperature resistant Polyimide (PAA) adhesive solution with the solid content of 22 percent.
Example 3
The high temperature resistant adhesive and the flexible copper clad laminate prepared by the high temperature resistant adhesive are prepared by stirring, dissolving and mixing Polyimide (PAA) adhesive solution with the solid content of 22 percent according to the weight proportion of polyimide resin, JER-1256 ultrahigh molecular weight epoxy resin, OP-935 flame retardant and DMAC dimethylacetamide; then coating a Polyimide (PAA) adhesive solution on a Polyimide (PI) film to prepare the adhesive-free flexible copper clad laminate with a high Tg (glass transition temperature) point.
The method for preparing the high-temperature resistant Polyimide (PAA) adhesive from the components in proportion comprises the following steps:
(1) Preparation of polyimide solution
Respectively weighing the polyimide resin powder 19 and the DMAC dimethylacetamide 71.3 according to the weight ratio, putting the materials into a stirring tank together, and stirring the materials at a high speed for 120 minutes to prepare a polyimide solution;
(2) Preparation of high temperature resistant adhesive
Respectively weighing 0.9 parts of JER-1256 ultrahigh molecular weight epoxy resin and 3.2 parts of OP-935 flame retardant, placing into a stirring tank, stirring at high speed for 120 minutes, and fully mixing with the polyimide solution to prepare the high temperature resistant Polyimide (PAA) adhesive solution with the solid content of 22 percent.
Example 4
The high-temperature-resistant adhesive and the flexible copper clad laminate prepared by the high-temperature-resistant adhesive are prepared by stirring, dissolving and mixing Polyimide (PAA) adhesive solution with the solid content of 22% according to the weight ratio of polyimide resin, JER-1256 ultrahigh molecular weight epoxy resin, OP-935 flame retardant and DMAC dimethylacetamide; then coating a Polyimide (PAA) adhesive solution on a Polyimide (PI) film to prepare the adhesive-free flexible copper clad laminate with a high Tg (glass transition temperature) point.
The method for preparing the high-temperature resistant Polyimide (PAA) adhesive from the components in proportion is as follows:
(1) Preparing polyimide solution
Respectively weighing the polyimide resin powder 21 and DMAC (dimethylacetamide) 64.4 according to the weight ratio, putting the weighed materials into a stirring tank, and stirring the materials at a high speed for 120 minutes to prepare a polyimide solution;
(2) Preparation of high temperature resistant adhesive
Respectively weighing the components in the weight ratio of JER-1256 ultra-high molecular weight epoxy resin 1.1 to OP-935 flame retardant 2.8, placing the mixture into a stirring tank, stirring the mixture for 120 minutes at a high speed, and fully mixing the mixture with polyimide solution to prepare high temperature resistant Polyimide (PAA) adhesive solution with the solid content of 22 percent.
Example 5
The high-temperature-resistant adhesive and the flexible copper clad laminate prepared by the high-temperature-resistant adhesive are prepared by stirring, dissolving and mixing Polyimide (PAA) adhesive solution with the solid content of 22% according to the weight ratio of polyimide resin, JER-1256 ultrahigh molecular weight epoxy resin, OP-935 flame retardant and DMAC dimethylacetamide; then coating a Polyimide (PAA) adhesive solution on a Polyimide (PI) film to prepare the adhesive-free flexible copper clad laminate with a high Tg (glass transition temperature) point.
The method for preparing the high-temperature resistant Polyimide (PAA) adhesive from the components in proportion is as follows:
(1) Preparing polyimide solution
Respectively weighing the polyimide resin powder 20 and the DMAC (dimethylacetamide) 68 according to the weight ratio, putting the materials into a stirring tank together, and stirring the materials at a high speed for 120 minutes to prepare a polyimide solution;
(2) Preparation of high temperature resistant adhesive
Respectively weighing the components in the weight ratio of the JER-1256 ultrahigh molecular weight epoxy resin 1 and the OP-935 flame retardant 3, putting the components into a stirring tank, stirring the components at a high speed for 120 minutes, and fully mixing the components with the polyimide solution to prepare the high temperature resistant Polyimide (PAA) adhesive solution with the solid content of 22 percent.
Claims (8)
1. A high temperature resistant adhesive and flexible copper clad laminate made of it, characterized by that by polyimide resin, JER-1256 ultra-high molecular weight epoxy resin, OP-935 fire retardant, DMAC dimethyl acetamide according to the weight proportion, through stirring and dissolving, stir and mix, make Polyimide (PAA) adhesive solution with 22% of the solid content; then coating a Polyimide (PAA) adhesive solution on a Polyimide (PI) film to prepare a non-adhesive flexible copper clad laminate with a high Tg (glass transition temperature) point; the method for preparing the high-temperature resistant Polyimide (PAA) adhesive solution comprises the following steps:
(1) Preparing polyimide solution
Respectively weighing the polyimide resin powder 16-24 and the DMAC dimethylacetamide 54.4-81.3 in parts by weight, putting the materials into a stirring tank together, and stirring the materials at a high speed for 120 minutes to prepare a polyimide solution;
(2) Preparation of high temperature resistant adhesive
Respectively weighing 0.8-1.2 parts by weight of JER-1256 ultra-high molecular weight epoxy resin and 2.4-3.6 parts by weight of OP-935 flame retardant, placing into a stirring tank, stirring at high speed for 120 minutes, and fully mixing with the polyimide solution to prepare the high-temperature resistant Polyimide (PAA) adhesive solution with the solid content of 22%.
2. The high temperature resistant adhesive and the flexible copper clad laminate made of the same according to claim 1, wherein the method for preparing the high temperature resistant Polyimide (PAA) adhesive solution is as follows:
(1) Preparing polyimide solution
Respectively weighing the polyimide resin powder 24 and the DMAC (dimethylacetamide) 54.4 according to the weight ratio, putting the weighed materials into a stirring tank, and stirring the materials at a high speed for 120 minutes to prepare a polyimide solution;
(2) Preparation of high temperature resistant adhesive
Respectively weighing the components in the weight ratio of JER-1256 ultra-high molecular weight epoxy resin 1.2 to OP-935 flame retardant 2.4, placing the mixture into a stirring tank, stirring the mixture for 120 minutes at a high speed, and fully mixing the mixture with polyimide solution to prepare high temperature resistant Polyimide (PAA) adhesive solution with the solid content of 22 percent.
3. The high temperature resistant adhesive and the flexible copper clad laminate made therefrom according to claim 1, wherein the method for preparing the high temperature resistant Polyimide (PAA) adhesive solution is as follows:
(1) Preparing polyimide solution
Respectively weighing the polyimide resin powder 16 and the DMAC (dimethylacetamide) 81.3 according to the weight ratio, putting the weighed materials into a stirring tank, and stirring the materials at a high speed for 120 minutes to prepare a polyimide solution;
(2) Preparation of high temperature resistant adhesive
Respectively weighing 0.8 parts of JER-1256 ultrahigh molecular weight epoxy resin and 3.6 parts of OP-935 flame retardant, placing into a stirring tank, stirring at high speed for 120 minutes, and fully mixing with the polyimide solution to prepare the high temperature resistant Polyimide (PAA) adhesive solution with the solid content of 22 percent.
4. The high temperature resistant adhesive and the flexible copper clad laminate made of the same according to claim 1, wherein the method for preparing the high temperature resistant Polyimide (PAA) adhesive solution is as follows:
(1) Preparation of polyimide solution
Respectively weighing the polyimide resin powder 19 and the DMAC dimethylacetamide 71.3 according to the weight ratio, putting the materials into a stirring tank together, and stirring the materials at a high speed for 120 minutes to prepare a polyimide solution;
(2) Preparation of high temperature resistant adhesive
Respectively weighing 0.9 parts of JER-1256 ultra-high molecular weight epoxy resin and 3.2 parts of OP-935 flame retardant, putting the materials into a stirring tank, stirring the materials at a high speed for 120 minutes, and fully mixing the materials with polyimide solution to prepare high-temperature resistant Polyimide (PAA) adhesive solution with the solid content of 22 percent.
5. The high temperature resistant adhesive and the flexible copper clad laminate made of the same according to claim 1, wherein the method for preparing the high temperature resistant Polyimide (PAA) adhesive solution is as follows:
(1) Preparation of polyimide solution
Respectively weighing the polyimide resin powder 21 and DMAC (dimethylacetamide) 64.4 according to the weight ratio, putting the weighed materials into a stirring tank, and stirring the materials at a high speed for 120 minutes to prepare a polyimide solution;
(2) Preparation of high temperature resistant adhesive
Respectively weighing the components in the weight ratio of JER-1256 ultra-high molecular weight epoxy resin 1.1 to OP-935 flame retardant 2.8, placing the mixture into a stirring tank, stirring the mixture for 120 minutes at a high speed, and fully mixing the mixture with polyimide solution to prepare high temperature resistant Polyimide (PAA) adhesive solution with the solid content of 22 percent.
6. The high temperature resistant adhesive and the flexible copper clad laminate made therefrom according to claim 1, wherein the method for preparing the high temperature resistant Polyimide (PAA) adhesive solution is as follows:
(1) Preparation of polyimide solution
Respectively weighing the polyimide resin powder 20 and the DMAC (dimethylacetamide) 68 according to the weight ratio, putting the materials into a stirring tank together, and stirring the materials at a high speed for 120 minutes to prepare a polyimide solution;
(2) Preparation of high temperature resistant adhesive
Respectively weighing the components according to the weight ratio of the JER-1256 ultrahigh molecular weight epoxy resin 1 to the OP-935 flame retardant 3, putting the components into a stirring tank, stirring the components at a high speed for 120 minutes, and fully mixing the components with the polyimide solution to prepare the high temperature resistant Polyimide (PAA) adhesive solution with the solid content of 22 percent.
7. The high temperature resistant adhesive and the flexible copper clad laminate made of the same according to claim 1, wherein EPM-420 multifunctional epoxy resin 8, 4' -DDS epoxy resin curing agent 1.2 and 2E4MZ promoter 0.06 are added during the preparation of the high temperature resistant adhesive, and the stirring is continued for 120 minutes to 360 minutes to prepare a Polyimide (PAA) adhesive solution with a solid content of 22%.
8. The high temperature resistant adhesive and the flexible copper clad laminate made therefrom according to claim 1, wherein the method for making the flexible copper clad laminate without adhesive by using the high temperature resistant Polyimide (PAA) adhesive comprises:
(1) Coating of
Placing and coating the prepared high-temperature-resistant Polyimide (PAA) adhesive solution on a Polyimide (PI) film, wherein the thickness of the coated dry adhesive is controlled to be 5-15 mu m;
(2) Drying the mixture
Placing the coated material into an oven for drying at 160 ℃ for 3 minutes and realizing partial crosslinking;
(3) Pressing together
Placing the dried material on the rough surface of the copper foil, then placing the materials into a coating machine together, and carrying out hot-pressing lamination under the conditions of 160 ℃ and 0.4KGF/cm < 2 > pressure to ensure that the dried material and the rough surface of the copper foil are linearly laminated;
(4) Curing
And (3) placing the laminated material into an oven, and curing for 180 minutes at 180 ℃ to obtain the adhesive-free flexible copper-clad plate with a high Tg (glass transition temperature) point.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211096062.8A CN115678488A (en) | 2022-09-08 | 2022-09-08 | High-temperature-resistant adhesive and flexible copper clad laminate prepared from same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211096062.8A CN115678488A (en) | 2022-09-08 | 2022-09-08 | High-temperature-resistant adhesive and flexible copper clad laminate prepared from same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115678488A true CN115678488A (en) | 2023-02-03 |
Family
ID=85062702
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211096062.8A Pending CN115678488A (en) | 2022-09-08 | 2022-09-08 | High-temperature-resistant adhesive and flexible copper clad laminate prepared from same |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115678488A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106800908A (en) * | 2016-12-27 | 2017-06-06 | 广东生益科技股份有限公司 | A kind of two-layer method flexibility coat copper plate TPI adhesive and preparation method thereof, application |
| CN109096979A (en) * | 2018-08-15 | 2018-12-28 | 南昌正业科技有限公司 | A kind of adhesive and a kind of flexibility coat copper plate with high glass-transition temperature |
| CN109266297A (en) * | 2018-09-18 | 2019-01-25 | 江西华莲欣科技有限公司 | A kind of high-temperature Resistance Adhesives and its preparation method and application |
| CN109379831A (en) * | 2018-09-18 | 2019-02-22 | 江西华莲欣科技有限公司 | A kind of thermoplastic polyimide type Rigid Flex and preparation method |
-
2022
- 2022-09-08 CN CN202211096062.8A patent/CN115678488A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106800908A (en) * | 2016-12-27 | 2017-06-06 | 广东生益科技股份有限公司 | A kind of two-layer method flexibility coat copper plate TPI adhesive and preparation method thereof, application |
| CN109096979A (en) * | 2018-08-15 | 2018-12-28 | 南昌正业科技有限公司 | A kind of adhesive and a kind of flexibility coat copper plate with high glass-transition temperature |
| CN109266297A (en) * | 2018-09-18 | 2019-01-25 | 江西华莲欣科技有限公司 | A kind of high-temperature Resistance Adhesives and its preparation method and application |
| CN109379831A (en) * | 2018-09-18 | 2019-02-22 | 江西华莲欣科技有限公司 | A kind of thermoplastic polyimide type Rigid Flex and preparation method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101550264A (en) | Resin matching fluid used for metal foil laminated board | |
| KR20160059286A (en) | Flexible metal laminate | |
| CN111867260A (en) | Coating forming method of novel material layer structure of high-frequency circuit board and product thereof | |
| CN115305031A (en) | Low-dielectric high-Tg hydrocarbon bonding sheet and high-frequency copper-clad plate prepared from same | |
| CN115710338A (en) | Benzoxazine resin for flexible non-adhesive copper-clad plate, benzoxazine monomer, preparation method and application thereof | |
| CN114015409A (en) | Composite adhesive, flexible copper-clad plate and preparation method thereof | |
| KR100823998B1 (en) | Copper clad laminate, printed circuit board and manufacturing method of ccl | |
| CN101600296B (en) | Polyimide copper clad lamination containing thioether structure and preparation method thereof | |
| CN115595105B (en) | Composite adhesive for copper-clad plate and preparation method thereof | |
| CN115678488A (en) | High-temperature-resistant adhesive and flexible copper clad laminate prepared from same | |
| CN111867242A (en) | Press-forming method of novel material layer structure of high-frequency circuit board and product thereof | |
| CN109233724B (en) | High-glass-transition-temperature adhesive and application thereof to covering film | |
| CN115028998B (en) | Preparation method of halogen-free low-loss copper-clad plate for high-frequency high-speed field | |
| CN114149659B (en) | Resin composition and use thereof | |
| CN111479395B (en) | Preparation method of glue-free flexible copper-clad plate | |
| CN108943895A (en) | Two layers of method double side flexible copper coated board of one kind and preparation method thereof | |
| CN101463115B (en) | Thermoset polyimide resin for non-gel flexible single-side coated copper plate and use thereof | |
| CN112373150A (en) | Preparation method of glue-free single-sided flexible copper-clad plate based on coating method | |
| CN102786771A (en) | Resin liquid, metal substrate adopting the resin liquid, and manufacturing method of the metal substrate | |
| CN111944274A (en) | Bendable prepreg gumming solution for circuit board, prepreg and preparation method of prepreg | |
| CN111662640A (en) | Modified liquid crystal material for 5G communication, copper-clad plate and preparation method thereof | |
| Tasaki | Low transmission loss polyimides substrates: a novel alternative to liquid crystal polymers | |
| CN102054706A (en) | Method for preparing incohesive flexible copper-clad plate from thermoplastic polyimide resin | |
| CN116333491B (en) | Halogen-free resin composition suitable for high-speed communication and application thereof | |
| CN104844801A (en) | Silicon-containing polyimide copper-clad plate and preparation 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 | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20230203 |