CN113022049A - Novel copper-clad plate structure and manufacturing process thereof - Google Patents
Novel copper-clad plate structure and manufacturing process thereof Download PDFInfo
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- CN113022049A CN113022049A CN202110327268.6A CN202110327268A CN113022049A CN 113022049 A CN113022049 A CN 113022049A CN 202110327268 A CN202110327268 A CN 202110327268A CN 113022049 A CN113022049 A CN 113022049A
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- epoxy resin
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- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 239000010410 layer Substances 0.000 claims abstract description 70
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 34
- 239000011159 matrix material Substances 0.000 claims abstract description 31
- 239000000835 fiber Substances 0.000 claims abstract description 29
- 239000000945 filler Substances 0.000 claims abstract description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004020 conductor Substances 0.000 claims abstract description 13
- 239000004593 Epoxy Substances 0.000 claims abstract description 12
- 238000009413 insulation Methods 0.000 claims abstract description 12
- 239000004831 Hot glue Substances 0.000 claims abstract description 11
- 229910052802 copper Inorganic materials 0.000 claims abstract description 11
- 239000010949 copper Substances 0.000 claims abstract description 11
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- 238000007731 hot pressing Methods 0.000 claims abstract description 6
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- 239000003822 epoxy resin Substances 0.000 claims description 38
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 17
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 16
- 125000003277 amino group Chemical group 0.000 claims description 15
- 229910052710 silicon Inorganic materials 0.000 claims description 14
- 239000010703 silicon Substances 0.000 claims description 14
- 239000000758 substrate Substances 0.000 claims description 10
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- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
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- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 9
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- 239000004278 EU approved seasoning Substances 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
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- 125000002029 aromatic hydrocarbon group Chemical group 0.000 claims description 3
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical class C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 230000005595 deprotonation Effects 0.000 claims description 3
- 238000010537 deprotonation reaction Methods 0.000 claims description 3
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 3
- 235000011194 food seasoning agent Nutrition 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 150000008442 polyphenolic compounds Chemical class 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- 150000004756 silanes Chemical class 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000004842 bisphenol F epoxy resin Substances 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 5
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- 230000014759 maintenance of location Effects 0.000 description 4
- JTWJUVSLJRLZFF-UHFFFAOYSA-N 2$l^{2},3$l^{2},4$l^{2},5$l^{2},6$l^{2},7$l^{2},8$l^{2},9$l^{2},11$l^{2},12$l^{2}-decaborabicyclo[8.1.1]dodecane Chemical compound [B]1C2[B]C1[B][B][B][B][B][B][B][B]2 JTWJUVSLJRLZFF-UHFFFAOYSA-N 0.000 description 3
- 239000011889 copper foil Substances 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 239000002313 adhesive film Substances 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- 150000004985 diamines Chemical class 0.000 description 2
- -1 m-aminophenyl Chemical group 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- LCLCCQZQBXFBNA-UHFFFAOYSA-N NCC(C=CC=C1)=C1[Si]C1=C(CN)C=CC=C1 Chemical compound NCC(C=CC=C1)=C1[Si]C1=C(CN)C=CC=C1 LCLCCQZQBXFBNA-UHFFFAOYSA-N 0.000 description 1
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000004113 Sepiolite Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- YCIVSJFIXXVSRH-UHFFFAOYSA-N amino-methyl-phenylsilicon Chemical compound C[Si](N)C1=CC=CC=C1 YCIVSJFIXXVSRH-UHFFFAOYSA-N 0.000 description 1
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- UKJLNMAFNRKWGR-UHFFFAOYSA-N cyclohexatrienamine Chemical group NC1=CC=C=C[CH]1 UKJLNMAFNRKWGR-UHFFFAOYSA-N 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000009432 framing Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
- B32B15/092—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising epoxy resins
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
- B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
- B32B27/26—Layered products comprising a layer of synthetic resin characterised by the use of special additives using curing agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/38—Layered products comprising a layer of synthetic resin comprising epoxy resins
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
- B32B3/02—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by features of form at particular places, e.g. in edge regions
- B32B3/08—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by features of form at particular places, e.g. in edge regions characterised by added members at particular parts
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
- B32B37/1207—Heat-activated adhesive
- B32B2037/1215—Hot-melt adhesive
Landscapes
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Laminated Bodies (AREA)
Abstract
The utility model provides a novel copper clad laminate structure, adopts hot-pressing technology preparation, wherein at least one deck insulating layer is located under the one deck conductor layer, adopt hot-pressing to consolidate between insulating layer and the conductor layer, be equipped with the glued layer between insulating layer and conductor layer, the glued layer contains three layer construction at least, and wherein at least one deck is the organosilicon insulation fiber pipe of vertical arrangement, is equipped with EVA hot melt adhesive layer on the two sides of organosilicon insulation fiber pipe, the insulating layer comprises filler, epoxy matrix and curing agent, filler, epoxy matrix and curing agent homogeneous mixing.
Description
Technical Field
The invention relates to the field of electronic materials, in particular to a novel copper-clad plate structure and a manufacturing process thereof.
Background
In the production cost constitution of the existing Copper Clad Laminate (CCL), the cost of most materials is difficult to reduce, and the aim of reducing the production cost is difficult to achieve. Taking the glass fiber epoxy substrate with the highest use ratio as an example, the raw materials account for about 70-80% of the production cost, and the rest are parts which are difficult to reduce such as manpower, water and electricity, depreciation and the like; in the cost of raw materials, the glass fiber cloth occupies more than four, the copper foil occupies nearly three, and the epoxy resin also occupies nearly three. The glass fiber cloth and the copper foil mainly depend on upstream raw material manufacturers, so that a small number of replaceable materials are available, and the cost of the glass fiber cloth and the copper foil cannot be reduced due to the fact that the international oil price is increased nowadays.
The EVA adhesive film is made up by using EVA as main film-forming material, adding various assistants, forming by means of casting process, placing the adhesive film into laminator, heating, pressurizing, vacuum-pumping and framing, and finally making into the invented component.
In the prior art, the copper-clad plate matrix has poor heat resistance, but the use temperature of common epoxy resin is generally not more than 200 ℃, so the copper-clad plate structure is not manufactured by a hot-press bonding process. The invention provides a novel copper clad plate structure manufactured by adopting a hot-press bonding process and a manufacturing process thereof.
Disclosure of Invention
The invention aims to provide a novel copper clad laminate structure and a manufacturing process thereof, which adopt high-temperature-resistant epoxy resin as a main matrix material and realize the process of producing the copper clad laminate by a hot-pressing technology.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the utility model provides a novel copper clad laminate structure, wherein at least one deck insulating layer is located under the one deck conductor layer, adopt hot bonding cementation between insulating layer and the conductor layer, be equipped with the cementation layer between insulating layer and conductor layer, the cementation layer contains three layer construction at least, and wherein at least one deck is vertical arrangement's organosilicon insulation fiber tubular structure, is equipped with EVA hot melt adhesive layer on the two sides of organosilicon insulation fiber tube structure, the insulating layer comprises filler, epoxy matrix and curing agent, filler, epoxy matrix and curing agent homogeneous mixing, weight percent content is between epoxy matrix and each component of filler:
epoxy resin matrix: 57.5 to 67.5 percent
Filling: 12.5 to 22.5 percent
Curing agent: 20 to 30 percent
Preferably, the organosilicon insulation fiber tube is of a solid cylindrical structure, a styrene-butadiene latex insulation layer is coated outside the organosilicon insulation fiber tube, and the diameter of the section of the organosilicon insulation fiber tube-shaped structure is 10-30 micrometers.
Preferably, the curing agent is an amino curing agent, the amino curing agent comprises a carborane group and an amino group, the amino curing agent comprises two amino groups, the two amino groups are respectively end groups of the amino curing agent, and the amino group is directly connected with the carborane group, or the amino group is respectively connected with the carborane group through an aromatic hydrocarbon structure, a silicon group or a silicon oxygen group.
Preferably, the epoxy resin matrix is selected from at least one of bisphenol a type epoxy resin, hydrogenated bisphenol a type epoxy resin, bisphenol F type epoxy resin, polyphenol type glycidyl ether epoxy resin, novolac epoxy resin, and hydrogenated novolac epoxy resin.
A manufacturing process of a novel copper-clad plate is characterized by comprising the following steps:
(1) in an inert protection atmosphere, dispersing carborane in an ether solvent to obtain a carborane solution;
(2) cooling the carborane solution to-70-40 ℃, adding a metal deprotonation reagent into the solution, and reacting at room temperature to obtain a first intermediate;
(3) adding halogenated silane or halogenated siloxane into the solution, and carrying out reflux reaction on the first intermediate and the silane or siloxane at the temperature of 30-40 ℃ to obtain a second intermediate;
(4) cooling the solution to-30-10 ℃, introducing ammonia gas into the solution, and reacting to obtain the amino curing agent;
(5) mixing the amino curing agent, an epoxy resin matrix and seasonings according to a ratio to obtain the insulating layer matrix;
(6) coating a styrene-butadiene latex insulating layer outside the organic silicon insulating fiber pipe in a melting and precipitating way;
(7) placing the substrate in a vacuum box, laying an EVA hot-melt adhesive layer, an organic silicon insulating fiber tubular structure layer and an EVA hot-melt adhesive layer on the substrate in sequence, and applying certain pressure to evacuate air in the substrate;
(8) and moving the plate-shaped structure after exhausting into a hot press for pressing, wherein the unit pressure is 30Mpa, the temperature is 180 ℃, the duration is 150 minutes, and cooling along with room temperature after finishing the pressing to obtain the novel copper-clad plate structure.
Drawings
FIG. 1 is a schematic view of the structure of the present invention.
FIG. 2 is a graph showing the thermal weight loss of the epoxy resin of the present invention in an air atmosphere.
Illustration of the drawings: 1-a conductor layer; 2-EVA hot melt adhesive layer; 3-an organic silicon insulating fiber tube; 4-an insulating layer.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Examples
The utility model provides a novel copper clad laminate structure, wherein at least one deck insulating layer 4 is located under one deck conductor layer 1, adopt hot pressing cementation between insulating layer 4 and the conductor layer 1, be equipped with the cementation layer between insulating layer 4 and conductor layer 1, the cementation layer contains three layer construction at least, and wherein at least one deck is vertical arrangement's organosilicon insulation fiber tube 3, is equipped with EVA hot melt adhesive layer 2 on organosilicon insulation fiber tube 3's two sides, insulating layer 4 comprises filler, epoxy matrix and curing agent, filler, epoxy matrix and curing agent homogeneous mixing, weight percent content is between epoxy matrix and each component of filler:
epoxy resin matrix: 57.5 to 67.5 percent
Filling: 12.5 to 22.5 percent
Curing agent: 20 to 30 percent
The curing agent is an amino curing agent which comprises carborane group and amino group, wherein the amino curing agent comprises two amino groups, the two amino groups are respectively terminal groups of the amino curing agent, and the amino groups are directly connected with the carborane group, or the amino groups are respectively connected with the carborane group through aromatic hydrocarbon structures, silicon groups or silicon oxygen groups.
The epoxy resin matrix is selected from at least one of bisphenol A epoxy resin, hydrogenated bisphenol A epoxy resin, bisphenol F epoxy resin, polyphenol glycidyl ether epoxy resin, novolac epoxy resin and hydrogenated novolac epoxy resin.
The following data were obtained experimentally, as shown in fig. 1:
the phenolic epoxy resin F51 is used as an epoxy resin matrix, the diamine meta-carborane of the A structure is used as a curing agent, the components are mixed according to the mass ratio of 100:20 of the F51 to the diamine meta-carborane of the A structure, and after curing is carried out for 2 hours at 180 ℃, the high-temperature resistant epoxy resin cured product is obtained.
The thermal weight loss of the cured product is tested in an air atmosphere: the mass retention at 800 ℃ was 76% (curve e in FIG. 2).
According to the bonding strength test, the bonding strength of the cured epoxy resin is 14.5MPa at room temperature, and the bonding strength after aging for 1 hour in the air at 600 ℃ is 2.8 MPa.
The phenolic epoxy resin F44 is used as an epoxy resin matrix, the bis (m-aminophenyl) m-carborane in the B structure is used as a curing agent, the components are mixed according to the mass ratio of the F44 to the bis (m-aminophenyl) m-carborane of 100:50, and after curing is carried out for 4 hours at 160 ℃, a high-temperature-resistant epoxy resin cured product is obtained.
The thermal weight loss of the cured product is tested in an air atmosphere: the mass retention at 800 ℃ was 71% (curve d in FIG. 2).
According to the bonding strength test, the bonding strength of the cured epoxy resin is 15.8MPa at room temperature, and the bonding strength after aging for 1 hour in the air at 600 ℃ is 2.6 MPa.
Bisphenol A epoxy resin E51 is used as an epoxy resin matrix, bis (amino methyl phenyl silicon-based) meta-carborane in a C structure is used as a curing agent, the mixture is mixed according to the mass ratio of E51 to bis (amino methyl phenyl) silicon-based carborane of 100:120, and after the mixture is cured for 5 hours at 150 ℃, the high-temperature resistant epoxy resin cured product is obtained.
The thermal weight loss of the cured product is tested in an air atmosphere: the mass retention at 800 ℃ was 60% (curve b in FIG. 2).
According to the bonding strength test, the bonding strength of the cured epoxy resin at room temperature is 16.8MPa, and the bonding strength after aging in the air at 600 ℃ for 1h is 2.1 MPa.
Mixing phenolic epoxy resin F51 and multifunctional epoxy resin AG80 according to the mass ratio of 80:20 to obtain an epoxy resin matrix, mixing the mixed epoxy resin and bis (p-aminophenyl) m-carborane in the structure B as a curing agent according to the mass ratio of 100:80, and curing at 120 ℃ for 8 hours to obtain a high-temperature-resistant epoxy resin cured product.
The thermal weight loss of the cured product is tested in an air atmosphere: the mass retention at 800 ℃ was 64% (curve c in FIG. 2).
According to the bonding strength test, the bonding strength of the cured epoxy resin at room temperature is 18.2MPa, and the bonding strength after aging in the air at 600 ℃ for 1h is 2.9 MPa.
In summary, the matrix made of the epoxy resin has good thermal stability.
The filler is an inorganic powder filler, the diameter of the powder is 5-10 microns, the powder is selected from at least one or more of alumina powder, magnesia powder, magnesium hydroxide powder, aluminum hydroxide powder, chalk powder, layered silicate powder, barite powder, sepiolite powder, talcum powder and mica powder, and the mechanical benefit of the epoxy resin matrix is further enhanced by the filler with the diameter of 5-10 microns.
The organic silicon insulating fiber tube is of a solid cylindrical structure, a styrene-butadiene latex insulating layer is coated outside the organic silicon insulating fiber tube, the diameter of the section of the organic silicon insulating fiber tube-shaped structure is 10-30 micrometers, and the thickness of the styrene-butadiene latex insulating layer coated on the organic silicon insulating fiber tube-shaped structure is 15-35 micrometers. The organosilicon insulating fiber tube has good electrical insulating property, the dielectric loss, the voltage resistance, the electric arc resistance, the corona resistance, the volume resistivity, the surface resistivity and the like of the organosilicon insulating fiber tube are listed in the insulating material, the outside of the organosilicon insulating fiber tube is coated with a styrene-butadiene latex insulating layer in a melting deposition mode, the insulating property of the fiber tube is further enhanced by the styrene-butadiene latex insulating layer, and the coating and parallel connection effects can be achieved.
A manufacturing process of a novel copper-clad plate comprises the following steps:
(1) in an inert protection atmosphere, dispersing carborane in an ether solvent to obtain a carborane solution;
(2) cooling the carborane solution to-70-40 ℃, adding a metal deprotonation reagent into the solution, and reacting at room temperature to obtain a first intermediate;
(3) adding halogenated silane or halogenated siloxane into the solution, and carrying out reflux reaction on the first intermediate and the silane or siloxane at the temperature of 30-40 ℃ to obtain a second intermediate;
(4) cooling the solution to-30-10 ℃, introducing ammonia gas into the solution, and reacting to obtain the amino curing agent;
(5) mixing the amino curing agent, an epoxy resin matrix and seasonings according to a ratio to obtain the insulating layer matrix;
(6) coating a styrene-butadiene latex insulating layer outside the organic silicon insulating fiber pipe in a melting and precipitating way;
(7) placing the substrate in a vacuum box, laying an EVA hot-melt adhesive layer, an organic silicon insulating fiber tubular structure layer and an EVA hot-melt adhesive layer on the substrate in sequence, and applying certain pressure to evacuate air in the substrate;
(8) and moving the plate-shaped structure after exhausting into a hot press for hot-press bonding and cementing, wherein the unit pressure is MPa, the temperature is 180 ℃, the duration is 150 minutes, and cooling along with room temperature after finishing the operation to obtain the novel copper-clad plate structure.
By adopting the method, the copper-clad plate can be manufactured by adopting a hot-pressing process, and the copper-clad plate has excellent economic value and certain performance.
The invention is well implemented in accordance with the above-described embodiments. It should be noted that, based on the above structural design, in order to solve the same technical problems, even if some insubstantial modifications or colorings are made on the present invention, the adopted technical solution is still the same as the present invention, and therefore, the technical solution should be within the protection scope of the present invention.
Claims (5)
1. A novel copper clad laminate structure, wherein at least one layer of insulating layer (4) is located under one layer of conductor layer (1), its characterized in that: adopt the hot-pressing cementation between insulating layer and conductor layer (1), be equipped with the cementation layer between insulating layer (4) and conductor layer (1), the cementation layer contains three layer construction at least, and wherein at least one deck is vertical arrangement's organosilicon insulation fiber pipe (3), is equipped with EVA hot melt adhesive layer (2) on the two sides of organosilicon insulation fiber pipe (3), insulating layer (4) comprise filler, epoxy matrix and curing agent, filler, epoxy matrix and curing agent homogeneous mixing, weight percent content is between epoxy matrix and each component of filler: epoxy resin matrix: 57.5% -67.5%, filler: 12.5% -22.5%, curing agent: 20 to 30 percent.
2. The novel copper clad laminate structure of claim 1, wherein: the organic silicon insulating fiber tube (3) is of a solid cylindrical structure, a styrene-butadiene latex insulating layer is coated outside the organic silicon insulating fiber tube (3), and the diameter of the section of the organic silicon insulating fiber tube (3) is 10-30 micrometers.
3. The novel copper clad laminate structure of claim 1, wherein: the curing agent is an amino curing agent which comprises carborane group and amino group, wherein the amino curing agent comprises two amino groups, the two amino groups are respectively terminal groups of the amino curing agent, and the amino groups are directly connected with the carborane group, or the amino groups are respectively connected with the carborane group through aromatic hydrocarbon structures, silicon groups or silicon oxygen groups.
4. The novel copper clad laminate structure of claim 1, wherein: the epoxy resin matrix is selected from at least one of bisphenol A epoxy resin, hydrogenated bisphenol A epoxy resin, bisphenol F epoxy resin, polyphenol glycidyl ether epoxy resin, novolac epoxy resin and hydrogenated novolac epoxy resin.
5. A manufacturing process of a novel copper-clad plate is characterized by comprising the following steps:
(1) in an inert protection atmosphere, dispersing carborane in an ether solvent to obtain a carborane solution;
(2) cooling the carborane solution to-70-40 ℃, adding a metal deprotonation reagent into the solution, and reacting at room temperature to obtain a first intermediate;
(3) adding halogenated silane or halogenated siloxane into the solution, and carrying out reflux reaction on the first intermediate and the silane or siloxane at the temperature of 30-40 ℃ to obtain a second intermediate;
(4) cooling the solution to-30-10 ℃, introducing ammonia gas into the solution, and reacting to obtain the amino curing agent;
(5) mixing the amino curing agent, an epoxy resin matrix and seasonings according to a ratio to obtain the insulating layer matrix;
(6) coating a styrene-butadiene latex insulating layer outside the organic silicon insulating fiber pipe in a melting and precipitating way;
(7) placing the substrate in a vacuum box, laying an EVA hot-melt adhesive layer, an organic silicon insulating fiber tubular structure layer and an EVA hot-melt adhesive layer on the substrate in sequence, and applying certain pressure to evacuate air in the substrate;
(8) and moving the plate-shaped structure after exhausting into a hot press for hot-press bonding and cementing, wherein the unit pressure is MPa, the temperature is 180 ℃, the duration is 150 minutes, and cooling along with room temperature after finishing the operation to obtain the novel copper-clad plate structure.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113477558A (en) * | 2021-06-27 | 2021-10-08 | 重庆德凯实业股份有限公司 | Device for producing and classifying and packaging copper-clad plates |
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Application publication date: 20210625 |