CN114025516B - Manufacturing method of high-frequency mixed pressing plate - Google Patents
Manufacturing method of high-frequency mixed pressing plate Download PDFInfo
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- CN114025516B CN114025516B CN202111398722.3A CN202111398722A CN114025516B CN 114025516 B CN114025516 B CN 114025516B CN 202111398722 A CN202111398722 A CN 202111398722A CN 114025516 B CN114025516 B CN 114025516B
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- ditelluride
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- hydrocarbon resin
- circuit board
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 238000003825 pressing Methods 0.000 title abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 53
- 239000000758 substrate Substances 0.000 claims abstract description 21
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052802 copper Inorganic materials 0.000 claims abstract description 15
- 239000010949 copper Substances 0.000 claims abstract description 15
- 238000007747 plating Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000007731 hot pressing Methods 0.000 claims abstract description 11
- 238000005530 etching Methods 0.000 claims abstract description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 142
- JPIIVHIVGGOMMV-UHFFFAOYSA-N ditellurium Chemical compound [Te]=[Te] JPIIVHIVGGOMMV-UHFFFAOYSA-N 0.000 claims description 88
- 229910052759 nickel Inorganic materials 0.000 claims description 71
- 239000013032 Hydrocarbon resin Substances 0.000 claims description 54
- 229920006270 hydrocarbon resin Polymers 0.000 claims description 54
- 229920000734 polysilsesquioxane polymer Polymers 0.000 claims description 35
- 239000011858 nanopowder Substances 0.000 claims description 32
- 238000003756 stirring Methods 0.000 claims description 21
- 239000011259 mixed solution Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- FPAYQPSNSPNOGF-UHFFFAOYSA-N [Ni]C=C Chemical compound [Ni]C=C FPAYQPSNSPNOGF-UHFFFAOYSA-N 0.000 claims description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 15
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 12
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000000919 ceramic Substances 0.000 claims description 8
- 238000013329 compounding Methods 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 239000004793 Polystyrene Substances 0.000 claims description 7
- 229920006026 co-polymeric resin Polymers 0.000 claims description 7
- 229920002223 polystyrene Polymers 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 5
- 238000009713 electroplating Methods 0.000 claims description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000005062 Polybutadiene Substances 0.000 claims description 4
- 229920001153 Polydicyclopentadiene Polymers 0.000 claims description 4
- 229920002857 polybutadiene Polymers 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 239000002174 Styrene-butadiene Substances 0.000 claims description 2
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 claims description 2
- 239000011115 styrene butadiene Substances 0.000 claims description 2
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 abstract description 4
- 238000005520 cutting process Methods 0.000 abstract description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 5
- 230000009477 glass transition Effects 0.000 description 4
- 238000004891 communication Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/46—Manufacturing multilayer circuits
- H05K3/4611—Manufacturing multilayer circuits by laminating two or more circuit boards
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F230/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
- C08F230/04—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal
- C08F230/08—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon
- C08F230/085—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon the monomer being a polymerisable silane, e.g. (meth)acryloyloxy trialkoxy silanes or vinyl trialkoxysilanes
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/0213—Electrical arrangements not otherwise provided for
- H05K1/0237—High frequency adaptations
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0306—Inorganic insulating substrates, e.g. ceramic, glass
Landscapes
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Laminated Bodies (AREA)
- Manufacturing Of Printed Wiring (AREA)
Abstract
The invention discloses a manufacturing method of a high-frequency mixed pressing plate, which comprises the following steps: step1, cleaning and drying a substrate, cutting the substrate into a proper shape, and then plating copper and etching to form a circuit pattern to obtain a circuit board; step 2, preparing an upper circuit board and a lower circuit board, and preparing two prepregs and a high-frequency material layer for later use; step 3, firstly, paving a lower circuit board on a flat tabletop, and then paving a first prepreg, a high-frequency material layer, a second prepreg and an upper circuit board on the surface of the lower circuit in sequence to obtain a to-be-pressed plate; and step 4, carrying out hot pressing treatment on the to-be-pressed plate by using a hydraulic press to obtain the high-frequency mixed pressing plate. The invention discloses a manufacturing method of a high-frequency mixed pressing plate, which is simple and easy to operate and has better high-temperature resistance, adhesiveness and dielectric property compared with the traditional manufacturing method.
Description
Technical Field
The invention relates to the field of high-frequency mixed pressing plates, in particular to a manufacturing method of a high-frequency mixed pressing plate.
Background
At present, electronic products are developed towards the high frequency and high speed digitization of signal transmission, the technology of the high frequency mixed pressing plate for 5G communication equipment is also greatly developed, the electronic products are changed more gradually, and the electronic products continuously tend to be developed in light, thin, short, small and high frequency, so that the requirements on the loaded circuit board are also higher and higher. Compared with the common FR4 circuit board material, the high-frequency mixed board for the 5G communication equipment is also called a special circuit board with higher electromagnetic frequency because the high-frequency material layer is mixed and pressed in the high-frequency mixed board.
In the manufacturing method, a mode of a double-layer circuit board is generally adopted as the high-frequency mixed board for the 5G communication equipment, namely, a high-frequency material layer is arranged between two layers of circuit boards, and the high-frequency material layer and the two layers of circuit boards are bonded through insulating prepregs, so that a complete high-frequency mixed board is formed. One of the commonly used high-frequency materials at present is hydrocarbon resin, however, the hydrocarbon resin has excellent dielectric properties, but has low glass transition temperature and poor heat resistance, a large amount of heat can be inevitably generated in the working and running process of the high-frequency mixed board, and the heat is transferred to a high-frequency material layer prepared from the hydrocarbon resin through a prepreg, so that the high-frequency material layer is easily burnt, the service life of the high-frequency mixed board is shortened, and the use cost of the high-frequency mixed board is increased.
Disclosure of Invention
Aiming at the problems that in the prior art, during the working and running of the high-frequency mixed pressing plate, heat is transferred to the high-frequency material layer through the prepreg, so that the high-frequency material layer is easy to burn, the service life of the high-frequency mixed pressing plate is shortened, and the use cost of the high-frequency mixed pressing plate is increased, the invention provides a manufacturing method of the high-frequency mixed pressing plate.
The aim of the invention is realized by adopting the following technical scheme:
The manufacturing method of the high-frequency mixed pressure plate comprises the following steps:
step 1, after a substrate is cleaned and dried and cut into a proper shape, copper plating layers are formed on two sides of the substrate, and then etching is performed on the surfaces of the two copper plating layers to form a circuit pattern, so that the circuit board is obtained;
step 2, preparing two circuit boards prepared in the step 1 as an upper circuit board and a lower circuit board respectively, and preparing two prepregs and a high-frequency material layer for later use;
step 3, firstly, paving a lower circuit board on a flat tabletop, and then paving a first prepreg, a high-frequency material layer, a second prepreg and an upper circuit board on the surface of the lower circuit in sequence to obtain a to-be-pressed plate;
and step 4, carrying out hot pressing treatment on the to-be-pressed plate by using a hydraulic press to obtain the high-frequency mixed pressing plate.
Preferably, in the step 1, the substrate is made of ceramic, and the thickness of the substrate is 0.35-0.55 mm.
Preferably, in the step 1, the copper plating layers are formed on the surface of the substrate by a combination of deposition and electroplating, and each copper plating layer has a thickness of 0.035 to 0.05mm.
Preferably, in the step 2, the sizes, materials and shapes of the two prepregs are the same.
Preferably, in the step 2, the high-frequency material layer is made of modified hydrocarbon resin, and the thickness of the high-frequency material layer is 0.1-0.5 mm.
Preferably, in the step 3, the thickness of each prepreg is 0.05-0.08 mm.
Preferably, in the step 4, the hot pressing process is as follows: heating the first section of the hydraulic press to 130-140 ℃, and carrying out heat preservation treatment for 0.5-1 h under normal pressure; then the second stage is heated to 150-180 ℃ and the heat preservation is carried out for 0.3-0.8 h under the condition that the pressure is 0.5-1 MPa; then the third section is heated to 200-250 ℃ and is heat-preserved for 2-5 h under the pressure of 6-8 MPa; finally, the temperature is reduced to room temperature under normal pressure.
Preferably, the modified hydrocarbon resin is obtained by compounding nickel ditelluride/cage polysilsesquioxane copolymer with hydrocarbon resin.
Preferably, the preparation process of the modified hydrocarbon resin comprises the following steps:
Dispersing nickel ditelluride/cage type polysilsesquioxane copolymer and hydrocarbon resin into an organic solvent, stirring and dispersing uniformly, and removing the solvent under reduced pressure to obtain modified hydrocarbon resin; wherein the mass ratio of the nickel ditelluride/cage polysilsesquioxane copolymer, the hydrocarbon resin and the organic solvent is 1:18-25:10-20.
Preferably, the organic solvent is at least one of acetone, toluene, xylene, 1, 4-dioxane, N-dimethylformamide, and N, N-dimethylacetamide.
Preferably, the hydrocarbon resin comprises one of styrene-butadiene resin, polystyrene, polydicyclopentadiene, polybutadiene.
Preferably, the preparation method of the nickel ditelluride/cage polysilsesquioxane copolymer comprises the following steps:
S1, weighing nickel ditelluride nano powder and vinyl trimethoxy silane, adding the nickel ditelluride nano powder and the vinyl trimethoxy silane into an ethanol water solution, and uniformly dispersing the mixture by ultrasonic to obtain nickel ditelluride mixed solution; wherein the mass fraction of the ethanol aqueous solution is 50-70%, and the mass ratio of the nickel ditelluride nano powder to the vinyl trimethoxy silane is 1:3-5:10-20;
S2, pouring the nickel ditelluride mixed solution into a reflux condensing device, starting stirring, dropwise adding 15-20% ammonia water into the nickel ditelluride mixed solution, heating to 45-55 ℃ after the dropwise adding is finished, continuously stirring for 8-10 h, cooling, filtering and drying to obtain vinyl nickel ditelluride nano powder; wherein the mass ratio of the ammonia water to the nickel ditelluride mixed solution is 1:5-10;
S2, weighing octavinyl-POSS and mixing with 1, 4-dioxane, adding vinyl nickel ditelluride nano powder after fully and uniformly mixing, fully mixing again, adding azodiisobutyronitrile, heating to 45-65 ℃, stirring for reaction for 6-8 hours, cooling to room temperature, filtering, washing the obtained solid with methanol for three times, and drying to obtain the nickel ditelluride/cage-type polysilsesquioxane copolymer; wherein the mass ratio of the octavinyl-POSS, the vinyl nickel ditelluride nano powder, the azodiisobutyronitrile and the 1, 4-dioxane is 1:0.6-0.8:0.03-0.05:20-30.
The beneficial effects of the invention are as follows:
the invention discloses a manufacturing method of a high-frequency mixed pressing plate, which is simple and easy to operate and has better high-temperature resistance, adhesiveness and dielectric property compared with the traditional manufacturing method.
In order to avoid the problem that the high-frequency material layer is easy to damage when a large amount of heat is transmitted, the material of the high-frequency material layer is modified, and the modification is based on the existing hydrocarbon resin. The modified hydrocarbon resin is prepared by compounding the nickel ditelluride/cage polysilsesquioxane copolymer and the hydrocarbon resin, so that the defects of low glass transition temperature and poor heat resistance of the hydrocarbon resin are overcome, the probability of burning high-frequency materials at high operating temperature is reduced, and the service life of the high-frequency mixed pressure plate is prolonged.
In addition, the modified hydrocarbon resin is prepared by compounding the nickel ditelluride/cage polysilsesquioxane copolymer and the hydrocarbon resin, so that the adhesive property and the dielectric property of the modified hydrocarbon resin serving as a high-frequency material are enhanced.
Detailed Description
The technical features, objects and advantages of the present invention will be more clearly understood from the following detailed description of the technical aspects of the present invention, but should not be construed as limiting the scope of the invention.
Hydrocarbon resin is a resin with all-hydrocarbon components, namely, the molecular structure of the hydrocarbon resin only contains C, H elements, and the molecular structure of the hydrocarbon resin does not contain polar groups, so that the hydrocarbon resin has excellent dielectric property, is often used as a high-frequency material, but has limited application due to the defects of low glass transition temperature and poor heat resistance.
In the invention, nickel ditelluride/cage polysilsesquioxane copolymer is added in the process of modifying hydrocarbon resin, and the nickel ditelluride/cage polysilsesquioxane copolymer is a product obtained by copolymerizing cage polysilsesquioxane on the basis of nickel ditelluride. Before the nickel ditelluride is compounded, the nickel ditelluride and vinyl silane are subjected to grafting reaction, and ammonia water increases the grafting efficiency of vinyl groups, so that the vinyl nickel ditelluride is obtained; the cage polysilsesquioxane is an olefin-based cage polysilsesquioxane prepared by using octavinyl-POSS and 1, 4-dioxane; then, copolymerizing vinyl nickel ditelluride and olefin-based cage polysilsesquioxane under the action of azodiisobutyronitrile to obtain the nickel ditelluride/cage polysilsesquioxane copolymer.
The invention is further described with reference to the following examples.
Example 1
The manufacturing method of the high-frequency mixed pressure plate comprises the following steps:
Step 1, cleaning and drying a ceramic substrate with the thickness of 0.4mm, cutting the ceramic substrate into a proper shape, forming copper plating layers with the thickness of 0.045mm on both sides of the substrate by a method of combining deposition and electroplating, and etching the surfaces of the two copper plating layers to form a circuit pattern to obtain the circuit board;
Step 2, preparing two circuit boards prepared in the step 1 as an upper circuit board and a lower circuit board respectively, and preparing two non-flowing PP sheets with the thickness of 0.06mm and the same size, material and shape and a high-frequency material layer with the thickness of 0.3mm for later use;
step 3, firstly, paving a lower circuit board on a flat tabletop, and then paving a first prepreg, a high-frequency material layer, a second prepreg and an upper circuit board on the surface of the lower circuit in sequence to obtain a to-be-pressed plate;
Step 4, carrying out hot pressing treatment on the to-be-pressed plate by using a hydraulic press, wherein the hot pressing treatment comprises the following steps: heating the first section of the hydraulic press to 135 ℃, and carrying out heat preservation treatment for 0.8h under normal pressure; then the second stage is heated to 165 ℃ and is heat-preserved for 0.5h under the condition that the pressure is 0.7 MPa; then the third section is heated to 220 ℃ and is heat-preserved for 3.5 hours under the condition of 7 MPa; finally, the temperature is reduced to room temperature under normal pressure, and the high-frequency mixed pressure plate is obtained.
In the step 2, the material of the high-frequency material layer is modified hydrocarbon resin, and the modified hydrocarbon resin is obtained by compounding nickel ditelluride/cage polysilsesquioxane copolymer and hydrocarbon resin.
The preparation process of the modified hydrocarbon resin comprises the following steps:
Dispersing nickel ditelluride/cage polysilsesquioxane copolymer and polystyrene into toluene, stirring and dispersing uniformly, and removing the solvent under reduced pressure to obtain modified hydrocarbon resin; wherein the mass ratio of nickel ditelluride/cage polysilsesquioxane copolymer, polystyrene and toluene is 1:22:15.
The preparation method of the nickel ditelluride/cage type polysilsesquioxane copolymer comprises the following steps:
S1, weighing nickel ditelluride nano powder and vinyl trimethoxy silane, adding the nickel ditelluride nano powder and the vinyl trimethoxy silane into an ethanol water solution, and uniformly dispersing the mixture by ultrasonic to obtain nickel ditelluride mixed solution; wherein the mass fraction of the ethanol aqueous solution is 60%, and the mass ratio of the nickel ditelluride nano powder to the vinyl trimethoxysilane to the ethanol aqueous solution is 1:4:15;
S2, pouring the nickel ditelluride mixed solution into a reflux condensing device, starting stirring, dropwise adding 15-20% ammonia water into the nickel ditelluride mixed solution, heating to 45-55 ℃ after the dropwise adding is finished, continuously stirring for 8-10 h, cooling, filtering and drying to obtain vinyl nickel ditelluride nano powder; wherein the mass ratio of the ammonia water to the nickel ditelluride mixed solution is 1:8;
S2, weighing octavinyl-POSS and mixing with 1, 4-dioxane, adding vinyl nickel ditelluride nano powder after fully and uniformly mixing, fully mixing again, adding azodiisobutyronitrile, heating to 45-65 ℃, stirring for reaction for 6-8 hours, cooling to room temperature, filtering, washing the obtained solid with methanol for three times, and drying to obtain the nickel ditelluride/cage-type polysilsesquioxane copolymer; wherein the mass ratio of the octavinyl-POSS, the vinyl nickel ditelluride nano powder, the azodiisobutyronitrile and the 1, 4-dioxane is 1:0.7:0.04:25.
Example 2
The manufacturing method of the high-frequency mixed pressure plate comprises the following steps:
Step 1, cleaning and drying a ceramic substrate with the thickness of 0.35mm, cutting the ceramic substrate into a proper shape, forming copper plating layers with the thickness of 0.035mm on both sides of the substrate by a method of combination of deposition and electroplating, and etching the surfaces of the two copper plating layers to form a circuit pattern to obtain a circuit board;
Step 2, preparing two circuit boards prepared in the step 1 as an upper circuit board and a lower circuit board respectively, and preparing two non-flowing PP sheets with the thickness of 0.05mm and the same size, material and shape and a high-frequency material layer with the thickness of 0.1mm for later use;
step 3, firstly, paving a lower circuit board on a flat tabletop, and then paving a first prepreg, a high-frequency material layer, a second prepreg and an upper circuit board on the surface of the lower circuit in sequence to obtain a to-be-pressed plate;
Step 4, carrying out hot pressing treatment on the to-be-pressed plate by using a hydraulic press, wherein the hot pressing treatment comprises the following steps: heating the first section of the hydraulic press to 130 ℃, and carrying out heat preservation treatment for 0.5h under normal pressure; then the second stage is heated to 150 ℃ and is heat-preserved for 0.3h under the condition of the pressure of 0.5 MPa; then the third section is heated to 200 ℃ and is heat-preserved for 2 hours under the condition of 6 MPa; finally, the temperature is reduced to room temperature under normal pressure, and the high-frequency mixed pressure plate is obtained.
In the step 2, the material of the high-frequency material layer is modified hydrocarbon resin, and the modified hydrocarbon resin is obtained by compounding nickel ditelluride/cage polysilsesquioxane copolymer and hydrocarbon resin.
The preparation process of the modified hydrocarbon resin comprises the following steps:
Dispersing nickel ditelluride/cage polysilsesquioxane copolymer and polydicyclopentadiene into dimethylbenzene, stirring and dispersing uniformly, and removing the solvent under reduced pressure to obtain modified hydrocarbon resin; wherein the mass ratio of nickel ditelluride/cage polysilsesquioxane copolymer, polydicyclopentadiene and dimethylbenzene is 1:18-25:10-20.
The preparation method of the nickel ditelluride/cage type polysilsesquioxane copolymer comprises the following steps:
S1, weighing nickel ditelluride nano powder and vinyl trimethoxy silane, adding the nickel ditelluride nano powder and the vinyl trimethoxy silane into an ethanol water solution, and uniformly dispersing the mixture by ultrasonic to obtain nickel ditelluride mixed solution; wherein the mass fraction of the ethanol aqueous solution is 50%, and the mass ratio of the nickel ditelluride nano powder to the vinyl trimethoxysilane to the ethanol aqueous solution is 1:3:10;
S2, pouring the nickel ditelluride mixed solution into a reflux condensing device, starting stirring, dropwise adding 15-20% ammonia water into the nickel ditelluride mixed solution, heating to 45-55 ℃ after the dropwise adding is finished, continuously stirring for 8-10 h, cooling, filtering and drying to obtain vinyl nickel ditelluride nano powder; wherein the mass ratio of the ammonia water to the nickel ditelluride mixed solution is 1:5;
S2, weighing octavinyl-POSS and mixing with 1, 4-dioxane, adding vinyl nickel ditelluride nano powder after fully and uniformly mixing, fully mixing again, adding azodiisobutyronitrile, heating to 45-65 ℃, stirring for reaction for 6-8 hours, cooling to room temperature, filtering, washing the obtained solid with methanol for three times, and drying to obtain the nickel ditelluride/cage-type polysilsesquioxane copolymer; wherein the mass ratio of the octavinyl-POSS, the vinyl nickel ditelluride nano powder, the azodiisobutyronitrile and the 1, 4-dioxane is 1:0.6:0.03:20.
Example 3
The manufacturing method of the high-frequency mixed pressure plate comprises the following steps:
Step 1, cleaning and drying a ceramic substrate with the thickness of 0.55mm, cutting the ceramic substrate into a proper shape, forming copper plating layers with the thickness of 0.05mm on both sides of the substrate by a method of combining deposition and electroplating, and etching the surfaces of the two copper plating layers to form a circuit pattern to obtain the circuit board;
Step 2, preparing two circuit boards prepared in the step 1 as an upper circuit board and a lower circuit board respectively, and preparing two non-flowing PP sheets with the thickness of 0.08mm and the same size, material and shape and a high-frequency material layer with the thickness of 0.5mm for later use;
step 3, firstly, paving a lower circuit board on a flat tabletop, and then paving a first prepreg, a high-frequency material layer, a second prepreg and an upper circuit board on the surface of the lower circuit in sequence to obtain a to-be-pressed plate;
Step 4, carrying out hot pressing treatment on the to-be-pressed plate by using a hydraulic press, wherein the hot pressing treatment comprises the following steps: heating the first section of the hydraulic press to 140 ℃, and carrying out heat preservation treatment for 1h under normal pressure; then the second stage is heated to 180 ℃ and is heat-preserved for 0.8h under the condition of the pressure of 1 MPa; then the third section is heated to 250 ℃ and is heat-preserved for 5 hours under the condition that the pressure is 8 MPa; finally, the temperature is reduced to room temperature under normal pressure, and the high-frequency mixed pressure plate is obtained.
In the step 2, the material of the high-frequency material layer is modified hydrocarbon resin, and the modified hydrocarbon resin is obtained by compounding nickel ditelluride/cage polysilsesquioxane copolymer and hydrocarbon resin.
The preparation process of the modified hydrocarbon resin comprises the following steps:
Dispersing nickel ditelluride/cage polysilsesquioxane copolymer and polybutadiene into N, N-dimethylformamide, stirring and dispersing uniformly, and removing the solvent under reduced pressure to obtain modified hydrocarbon resin; wherein the mass ratio of the nickel ditelluride/cage polysilsesquioxane copolymer, the polybutadiene and the N, N-dimethylformamide is 1:25:20.
The preparation method of the nickel ditelluride/cage type polysilsesquioxane copolymer comprises the following steps:
s1, weighing nickel ditelluride nano powder and vinyl trimethoxy silane, adding the nickel ditelluride nano powder and the vinyl trimethoxy silane into an ethanol water solution, and uniformly dispersing the mixture by ultrasonic to obtain nickel ditelluride mixed solution; wherein the mass fraction of the ethanol aqueous solution is 70%, and the mass ratio of the nickel ditelluride nano powder to the vinyl trimethoxysilane to the ethanol aqueous solution is 1:5:20;
S2, pouring the nickel ditelluride mixed solution into a reflux condensing device, starting stirring, dropwise adding 15-20% ammonia water into the nickel ditelluride mixed solution, heating to 45-55 ℃ after the dropwise adding is finished, continuously stirring for 8-10 h, cooling, filtering and drying to obtain vinyl nickel ditelluride nano powder; wherein the mass ratio of the ammonia water to the nickel ditelluride mixed solution is 1:10;
S2, weighing octavinyl-POSS and mixing with 1, 4-dioxane, adding vinyl nickel ditelluride nano powder after fully and uniformly mixing, fully mixing again, adding azodiisobutyronitrile, heating to 45-65 ℃, stirring for reaction for 6-8 hours, cooling to room temperature, filtering, washing the obtained solid with methanol for three times, and drying to obtain the nickel ditelluride/cage-type polysilsesquioxane copolymer; wherein the mass ratio of the octavinyl-POSS, the vinyl nickel ditelluride nano powder, the azodiisobutyronitrile and the 1, 4-dioxane is 1:0.8:0.05:30.
Comparative example 1
The high-frequency material layer is different from embodiment 1 in that:
The material of the high-frequency material layer is modified hydrocarbon resin, and the modified hydrocarbon resin is obtained by compounding nickel ditelluride/cage polysilsesquioxane copolymer and hydrocarbon resin.
The preparation process of the modified hydrocarbon resin comprises the following steps:
Dispersing nickel ditelluride nano powder and polystyrene into toluene, stirring and dispersing uniformly, and removing the solvent under reduced pressure to obtain modified hydrocarbon resin; wherein, the mass ratio of the nickel ditelluride nano powder to the polystyrene to the toluene is 1:22:15.
Comparative example 2
The high-frequency material layer is different from embodiment 1 in that: the material of the high-frequency material layer is polystyrene.
In order to more clearly illustrate the invention, the high-frequency material layers prepared in the examples 1-3 and the comparative examples 1-2 of the invention are subjected to performance detection and comparison, wherein the peel strength is detected according to a method of 2.4.8 in the test method specification IPC-TM-650; the dielectric constant is measured at 1GHz according to 2.5.5.9 method in test method specification IPC-TM-650; dielectric loss is the dielectric loss tangent at 1GHz as measured by 2.5.5.9 method in test method Specification IPC-TM-650.
The results are shown in Table 1:
TABLE 1 comparison of the Properties of different high frequency Material layers
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | |
| Glass transition temperature (. Degree. C.) | 176 | 182 | 169 | 121 | 106 |
| Peel strength (N/m) | 1.2 | 1.4 | 0.9 | 0.6 | 0.5 |
| Dielectric constant | 3.43 | 3.48 | 3.46 | 3.51 | 3.54 |
| Dielectric loss (. Times.10 -3) | 2.7 | 3.1 | 2.9 | 3.3 | 3.4 |
From examples 1 to 3, it is clear that the high-frequency material layer prepared by the invention has better performance even if different hydrocarbon resins are selected for modification; as is clear from examples 1 and comparative examples 1 to 2, the present invention has better properties than conventional hydrocarbon resins or general doped hydrocarbon resins, and is more suitable for use as a high-frequency material layer.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (9)
1. The manufacturing method of the high-frequency mixed pressure plate is characterized by comprising the following steps of:
step 1, after a substrate is cleaned and dried and cut into a proper shape, copper plating layers are formed on two sides of the substrate, and then etching is performed on the surfaces of the two copper plating layers to form a circuit pattern, so that the circuit board is obtained;
step 2, preparing two circuit boards prepared in the step 1 as an upper circuit board and a lower circuit board respectively, and preparing two prepregs and a high-frequency material layer for later use;
step 3, firstly, paving a lower circuit board on a flat tabletop, and then paving a first prepreg, a high-frequency material layer, a second prepreg and an upper circuit board on the surface of the lower circuit in sequence to obtain a to-be-pressed plate;
step 4, carrying out hot pressing treatment on the to-be-pressed plate by using a hydraulic press to obtain a high-frequency mixed pressed plate;
in the step 2, the material of the high-frequency material layer is modified hydrocarbon resin;
the modified hydrocarbon resin is obtained by compounding nickel ditelluride/cage polysilsesquioxane copolymer and hydrocarbon resin;
the preparation method of the nickel ditelluride/cage type polysilsesquioxane copolymer comprises the following steps:
S1, weighing nickel ditelluride nano powder and vinyl trimethoxy silane, adding the nickel ditelluride nano powder and the vinyl trimethoxy silane into an ethanol water solution, and uniformly dispersing the mixture by ultrasonic to obtain nickel ditelluride mixed solution; wherein the mass fraction of the ethanol aqueous solution is 50% -70%, and the mass ratio of the nickel ditelluride nano powder to the vinyl trimethoxysilane to the ethanol aqueous solution is 1:3-5:10-20;
S2, pouring the nickel ditelluride mixed solution into a reflux condensing device, starting stirring, dropwise adding 15-20% ammonia water into the nickel ditelluride mixed solution, heating to 45-55 ℃ after the dropwise adding is finished, continuously stirring for 8-10 hours, cooling, filtering and drying to obtain vinyl nickel ditelluride nano powder; wherein the mass ratio of the ammonia water to the nickel ditelluride mixed solution is 1:5-10;
S2, weighing octavinyl-POSS and mixing with 1, 4-dioxane, adding vinyl nickel ditelluride nano powder after fully and uniformly mixing, fully mixing again, adding azodiisobutyronitrile, heating to 45-65 ℃, stirring for reaction for 6-8 hours, cooling to room temperature, filtering, washing the obtained solid with methanol for three times, and drying to obtain the nickel ditelluride/cage-type polysilsesquioxane copolymer; wherein the mass ratio of the octavinyl-POSS, the vinyl nickel ditelluride nano powder, the azodiisobutyronitrile and the 1, 4-dioxane is 1:0.6-0.8:0.03-0.05:20-30.
2. The method for manufacturing a high-frequency hybrid board according to claim 1, wherein in the step 1, the substrate is made of ceramic, and the thickness of the substrate is 0.35-0.55 mm.
3. The method of claim 1, wherein in the step 1, the copper plating layers are formed on the surface of the substrate by a combination of deposition and electroplating, and each copper plating layer has a thickness of 0.035-0.05 mm.
4. The method for manufacturing a high-frequency hybrid board according to claim 1, wherein in the step 2, the sizes, materials and shapes of the two prepregs are the same.
5. The method of claim 1, wherein in the step 2, the thickness of the high-frequency material layer is 0.1-0.5 mm.
6. The method for manufacturing a high-frequency hybrid board according to claim 1, wherein in the step 3, the non-flowability PP sheets of the prepregs are 0.05-0.08 mm in thickness.
7. The method for manufacturing a high-frequency hybrid board according to claim 1, wherein in the step 4, the hot pressing process is as follows: heating the first section of the hydraulic press to 130-140 ℃, and carrying out heat preservation treatment for 0.5-1 h under normal pressure; then the second stage is heated to 150-180 ℃ and the heat preservation is carried out for 0.3-0.8 h under the condition that the pressure is 0.5-1 MPa; then the third section is heated to 200-250 ℃ and is subjected to heat preservation treatment for 2-5 h under the condition that the pressure is 6-8 MPa; finally, the temperature is reduced to room temperature under normal pressure.
8. The method for manufacturing the high-frequency hybrid board according to claim 1, wherein the preparation process of the modified hydrocarbon resin is as follows:
Dispersing nickel ditelluride/cage type polysilsesquioxane copolymer and hydrocarbon resin into an organic solvent, stirring and dispersing uniformly, and removing the solvent under reduced pressure to obtain modified hydrocarbon resin; wherein the mass ratio of the nickel ditelluride/cage polysilsesquioxane copolymer, the hydrocarbon resin and the organic solvent is 1:18-25:10-20.
9. The method for manufacturing a high-frequency hybrid board according to claim 1, wherein the hydrocarbon resin comprises one of styrene-butadiene resin, polystyrene, polydicyclopentadiene and polybutadiene.
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| CN110677983A (en) * | 2019-08-23 | 2020-01-10 | 李龙凯 | Press-forming method of novel material layer structure of high-frequency circuit board and product thereof |
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| LU101698B1 (en) * | 2020-03-18 | 2021-09-20 | Circuit Foil Luxembourg | Surface-treated copper foil for high-frequency circuit and method for producing same |
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| CN103188879A (en) * | 2011-12-29 | 2013-07-03 | 深圳玛斯兰电路科技实业发展有限公司 | Preparation method of inner layer of thick copper thin circuit board of printed circuit board |
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