CN114025516A - Method for manufacturing high-frequency mixing plate - Google Patents
Method for manufacturing high-frequency mixing plate Download PDFInfo
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- CN114025516A CN114025516A CN202111398722.3A CN202111398722A CN114025516A CN 114025516 A CN114025516 A CN 114025516A CN 202111398722 A CN202111398722 A CN 202111398722A CN 114025516 A CN114025516 A CN 114025516A
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- frequency
- circuit board
- ditelluride
- hydrocarbon resin
- nickel
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims description 21
- 238000002156 mixing Methods 0.000 title description 19
- 239000000463 material Substances 0.000 claims abstract description 55
- 239000000758 substrate Substances 0.000 claims abstract description 23
- 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
- 230000006835 compression Effects 0.000 claims abstract description 11
- 238000007906 compression Methods 0.000 claims abstract description 11
- 238000007731 hot pressing Methods 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 238000005520 cutting process Methods 0.000 claims abstract description 6
- 238000005530 etching Methods 0.000 claims abstract description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 118
- JPIIVHIVGGOMMV-UHFFFAOYSA-N ditellurium Chemical compound [Te]=[Te] JPIIVHIVGGOMMV-UHFFFAOYSA-N 0.000 claims description 68
- 229910052759 nickel Inorganic materials 0.000 claims description 59
- 239000013032 Hydrocarbon resin Substances 0.000 claims description 51
- 229920006270 hydrocarbon resin Polymers 0.000 claims description 51
- 229920000734 polysilsesquioxane polymer Polymers 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000004321 preservation Methods 0.000 claims description 15
- 239000000919 ceramic Substances 0.000 claims description 8
- 238000013329 compounding Methods 0.000 claims description 8
- 239000004793 Polystyrene Substances 0.000 claims description 7
- 229920002223 polystyrene Polymers 0.000 claims description 7
- 229920005989 resin Polymers 0.000 claims description 7
- 239000011347 resin Substances 0.000 claims description 7
- 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
- 239000003960 organic solvent Substances 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 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
- 239000011858 nanopowder Substances 0.000 description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 12
- 239000007788 liquid Substances 0.000 description 12
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 10
- 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 description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 8
- 238000001816 cooling Methods 0.000 description 8
- 238000001914 filtration Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- -1 vinyl ditelluride Chemical compound 0.000 description 8
- 229920002554 vinyl polymer Polymers 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 7
- FPAYQPSNSPNOGF-UHFFFAOYSA-N [Ni]C=C Chemical compound [Ni]C=C FPAYQPSNSPNOGF-UHFFFAOYSA-N 0.000 description 6
- 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
- 229920006026 co-polymeric resin Polymers 0.000 description 4
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 4
- 230000009477 glass transition Effects 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000001132 ultrasonic dispersion Methods 0.000 description 4
- 238000005406 washing Methods 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
- 125000003342 alkenyl group Chemical group 0.000 description 2
- 230000007547 defect Effects 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
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 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 compression plate, which comprises the following steps: step 1, cleaning and drying a substrate, cutting the substrate into a proper shape, plating copper and etching to form a circuit pattern, and obtaining a circuit board; step 2, preparing an upper circuit board and a lower circuit board, and then preparing two prepregs and a high-frequency material layer for standby; step 3, firstly, laying a lower circuit board on a flat desktop, and then sequentially laying a first prepreg, a high-frequency material layer, a second prepreg and an upper circuit board on the surface of the lower circuit board according to the sequence to obtain a board to be pressed; and 4, carrying out hot pressing treatment on the plate to be pressed by using a hydraulic machine to obtain the high-frequency mixed plate. The invention discloses a manufacturing method of a high-frequency mixed compression plate, the whole manufacturing method is simple and easy to operate, and compared with the traditional manufacturing method, the high-frequency mixed compression plate used by the invention has better high temperature resistance, adhesiveness and dielectric property.
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 signal transmission high-frequency and high-speed digitization, the technology of a high-frequency mixed-pressing plate for 5G communication equipment is also greatly developed, the electronic products change more and more day by day and tend to be light, thin, short, small and high-frequency continuously, and the requirements on a bearing circuit board are higher and higher. Compared with the common FR4 circuit board material, the high-frequency mixing board for 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 mixing board.
In terms of the manufacturing method, the high-frequency hybrid board for the 5G communication equipment generally adopts a double-layer circuit board mode, 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 an insulating prepreg, so that a complete high-frequency hybrid board is formed. One of the high-frequency materials commonly used at present is hydrocarbon resin, however, although the hydrocarbon resin has excellent dielectric properties, the glass transition temperature of the hydrocarbon resin is low, the heat resistance is poor, and a large amount of heat can be inevitably generated during the operation of the high-frequency hybrid board, and the heat is transferred to the high-frequency material layer prepared from the hydrocarbon resin through the prepreg, so that the high-frequency material layer is easily burnt, the service life of the high-frequency hybrid board is shortened, and the use cost of the high-frequency hybrid board is increased.
Disclosure of Invention
The invention provides a manufacturing method of a high-frequency hybrid board, aiming at the problems that in the prior art, heat is transferred to a high-frequency material layer through a prepreg during the working operation of the high-frequency hybrid board, so that the high-frequency material layer is easily burnt, the service life of the high-frequency hybrid board is shortened, and the use cost of the high-frequency hybrid board is increased.
The purpose of the invention is realized by adopting the following technical scheme:
a manufacturing method of a high-frequency mixed compression plate comprises the following steps:
step 1, cleaning and drying a substrate, cutting the substrate into a proper shape, forming copper plating layers on two surfaces of the substrate, and etching the surfaces of the two copper plating layers to form a circuit pattern, so as to obtain a circuit board;
step 2, preparing two circuit boards obtained 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, laying a lower circuit board on a flat desktop, and then sequentially laying a first prepreg, a high-frequency material layer, a second prepreg and an upper circuit board on the surface of the lower circuit board according to the sequence to obtain a board to be pressed;
and 4, carrying out hot pressing treatment on the plate to be pressed by using a hydraulic machine to obtain the high-frequency mixed 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 layer is formed on the surface of the substrate by a method combining deposition and electroplating, and the thickness of each copper plating layer is 0.035-0.05 mm.
Preferably, in step 2, the size, material and shape of the two prepregs are the same.
Preferably, in the step 2, the material of the high-frequency material layer is 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 of the non-flowing PP sheet of the prepreg is 0.05-0.08 mm.
Preferably, in the step 4, the hot pressing process includes: heating the first section of the hydraulic press to 130-140 ℃, and carrying out heat preservation treatment for 0.5-1 h at normal pressure; heating to 150-180 ℃ in the second stage, and carrying out heat preservation treatment for 0.3-0.8 h under the condition that the pressure is 0.5-1 MPa; then, the temperature is raised to 200-250 ℃ in the third section, and the heat preservation treatment is carried out for 2-5 h under the condition that the pressure is 6-8 MPa; and finally, reducing the temperature to room temperature under normal pressure.
Preferably, the modified hydrocarbon resin is obtained by compounding a nickel ditelluride/cage polysilsesquioxane copolymer with a hydrocarbon resin.
Preferably, the preparation process of the modified hydrocarbon resin is as follows:
dispersing the nickel ditelluride/cage polysilsesquioxane copolymer and the 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 to the hydrocarbon resin to 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 and 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 vinyl trimethoxy silane into an ethanol aqueous solution, and performing ultrasonic dispersion uniformly to obtain a nickel ditelluride mixed solution; wherein the mass fraction of the ethanol water solution is 50-70%, and the mass ratio of the nickel ditelluride nano powder, the vinyl trimethoxy silane and the ethanol water solution is 1: 3-5: 10-20;
s2, pouring the mixed liquid of the nickel ditelluride into a reflux condensing device, starting stirring, dropwise adding ammonia water with the mass fraction of 15-20% into the mixed liquid of the nickel ditelluride, after dropwise adding, heating to 45-55 ℃, continuously stirring for 8-10 h, cooling, filtering and drying to obtain vinyl nickel ditelluride nanopowder; wherein the mass ratio of the ammonia water to the mixed liquid of the nickel ditelluride is 1: 5-10;
s2, weighing octavinyl-POSS and 1, 4-dioxane, mixing, adding vinyl ditelluride nano powder after fully mixing, fully mixing again, adding azodiisobutyronitrile, heating to 45-65 ℃, stirring for reacting for 6-8 h, cooling to room temperature, filtering, washing the obtained solid with methanol for three times, and drying to obtain a nickel ditelluride/cage polysilsesquioxane copolymer; wherein the mass ratio of the octavinyl-POSS, the vinyl ditelluride nano powder, the azodiisobutyronitrile and the 1, 4-dioxane is 1: 0.6-0.8: 0.03-0.05: 20-30.
The invention has the beneficial effects that:
the invention discloses a manufacturing method of a high-frequency mixed compression plate, the whole manufacturing method is simple and easy to operate, and compared with the traditional manufacturing method, the high-frequency mixed compression plate used by the invention has better high temperature resistance, adhesiveness and dielectric property.
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 established on the basis of 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 out a high-frequency material at a high operation temperature is reduced, and the service life of the high-frequency mixed pressing plate is prolonged.
In addition, the modified hydrocarbon resin is prepared by compounding the nickel ditelluride/cage polysilsesquioxane copolymer with the hydrocarbon resin, and the adhesive property and the dielectric property of the high-frequency material are enhanced.
Detailed Description
For the purpose of more clearly illustrating the present invention and more clearly understanding the technical features, objects and advantages of the present invention, the technical solutions of the present invention will now be described in detail below, but are not to be construed as limiting the implementable scope of the present invention.
The hydrocarbon resin is a resin with full hydrocarbon components, namely, the molecular structure of the resin only contains C, H elements, and the molecular structure of the resin does not contain polar groups, so that the resin has excellent dielectric properties and is often used as a high-frequency material, but the application of the resin is limited due to the defects of low glass transition temperature and poor heat resistance.
In the process of modifying hydrocarbon resin, the ditelluride/cage polysilsesquioxane copolymer is added, and the ditelluride/cage polysilsesquioxane copolymer is a product obtained by copolymerizing cage polysilsesquioxane after being compounded on the basis of ditelluride. Wherein, before the nickel ditelluride is compounded, the nickel ditelluride is subjected to grafting reaction with vinyl silane, and the ammonia water increases the grafting efficiency of vinyl groups, so that the vinyl nickel ditelluride is obtained; the cage type polysilsesquioxane is an alkenyl cage type polysilsesquioxane prepared by using octavinyl-POSS and 1, 4-dioxane; and then carrying out copolymerization reaction on vinyl nickel ditelluride and alkenyl cage-type polysilsesquioxane under the action of azodiisobutyronitrile to finally obtain the nickel ditelluride/cage-type polysilsesquioxane copolymer.
The invention is further described below with reference to the following examples.
Example 1
A manufacturing method of a high-frequency mixed compression 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 two sides of the substrate by a method combining deposition and electroplating, and etching the surfaces of the two copper plating layers to form a circuit pattern, thus obtaining 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 0.06mm 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, laying a lower circuit board on a flat desktop, and then sequentially laying a first prepreg, a high-frequency material layer, a second prepreg and an upper circuit board on the surface of the lower circuit board according to the sequence to obtain a board to be pressed;
step 4, carrying out hot pressing treatment on the plate to be pressed by using a hydraulic press, specifically: heating the first section of the hydraulic press to 135 ℃, and carrying out heat preservation treatment for 0.8h under normal pressure; then the temperature is raised to 165 ℃ in the second stage, and the heat preservation treatment is carried out for 0.5h under the condition that the pressure is 0.7 MPa; then, the temperature is raised to 220 ℃ in the third section, and the heat preservation treatment is carried out for 3.5h under the condition that the pressure is 7 MPa; and finally, reducing the temperature to room temperature under normal pressure to obtain the high-frequency mixing plate.
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 a nickel ditelluride/cage type polysilsesquioxane copolymer and hydrocarbon resin.
The preparation process of the modified hydrocarbon resin comprises the following steps:
dispersing the 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 the nickel ditelluride/cage polysilsesquioxane copolymer to the polystyrene to the toluene is 1:22: 15.
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 vinyl trimethoxy silane into an ethanol aqueous solution, and performing ultrasonic dispersion uniformly to obtain a nickel ditelluride mixed solution; wherein the mass fraction of the ethanol aqueous solution is 60%, and the mass ratio of the nickel ditelluride nanopowder to the vinyltrimethoxysilane to the ethanol aqueous solution is 1:4: 15;
s2, pouring the mixed liquid of the nickel ditelluride into a reflux condensing device, starting stirring, dropwise adding ammonia water with the mass fraction of 15-20% into the mixed liquid of the nickel ditelluride, after dropwise adding, heating to 45-55 ℃, continuously stirring for 8-10 h, cooling, filtering and drying to obtain vinyl nickel ditelluride nanopowder; wherein the mass ratio of the ammonia water to the mixed liquid of the nickel ditelluride is 1: 8;
s2, weighing octavinyl-POSS and 1, 4-dioxane, mixing, adding vinyl ditelluride nano powder after fully mixing, fully mixing again, adding azodiisobutyronitrile, heating to 45-65 ℃, stirring for reacting for 6-8 h, cooling to room temperature, filtering, washing the obtained solid with methanol for three times, and drying to obtain a nickel ditelluride/cage polysilsesquioxane copolymer; wherein the mass ratio of the octavinyl-POSS, the vinyl ditelluride nano powder, the azodiisobutyronitrile and the 1, 4-dioxane is 1:0.7:0.04: 25.
Example 2
A manufacturing method of a high-frequency mixed compression 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 two surfaces of the substrate by a method combining deposition and electroplating, and etching the surfaces of the two copper plating layers to form a circuit pattern, thus obtaining a circuit board;
step 2, preparing two circuit boards obtained 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, laying a lower circuit board on a flat desktop, and then sequentially laying a first prepreg, a high-frequency material layer, a second prepreg and an upper circuit board on the surface of the lower circuit board according to the sequence to obtain a board to be pressed;
step 4, carrying out hot pressing treatment on the plate to be pressed by using a hydraulic press, specifically: 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 subjected to heat preservation treatment for 0.3h under the pressure of 0.5 MPa; then, the temperature is raised to 200 ℃ in the third section, and the heat preservation treatment is carried out for 2h under the condition that the pressure is 6 MPa; and finally, reducing the temperature to room temperature under normal pressure to obtain the high-frequency mixing plate.
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 a nickel ditelluride/cage type polysilsesquioxane copolymer and hydrocarbon resin.
The preparation process of the modified hydrocarbon resin comprises the following steps:
dispersing the 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 the nickel ditelluride/cage polysilsesquioxane copolymer, the polydicyclopentadiene and the dimethylbenzene is 1: 18-25: 10-20.
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 vinyl trimethoxy silane into an ethanol aqueous solution, and performing ultrasonic dispersion uniformly to obtain a nickel ditelluride mixed solution; wherein the mass fraction of the ethanol water solution is 50%, and the mass ratio of the nickel ditelluride nano powder to the vinyl trimethoxy silane to the ethanol water solution is 1:3: 10;
s2, pouring the mixed liquid of the nickel ditelluride into a reflux condensing device, starting stirring, dropwise adding ammonia water with the mass fraction of 15-20% into the mixed liquid of the nickel ditelluride, after dropwise adding, heating to 45-55 ℃, continuously stirring for 8-10 h, cooling, filtering and drying to obtain vinyl nickel ditelluride nanopowder; wherein the mass ratio of the ammonia water to the mixed liquid of the nickel ditelluride is 1: 5;
s2, weighing octavinyl-POSS and 1, 4-dioxane, mixing, adding vinyl ditelluride nano powder after fully mixing, fully mixing again, adding azodiisobutyronitrile, heating to 45-65 ℃, stirring for reacting for 6-8 h, cooling to room temperature, filtering, washing the obtained solid with methanol for three times, and drying to obtain a nickel ditelluride/cage polysilsesquioxane copolymer; wherein the mass ratio of the octavinyl-POSS, the vinyl ditelluride nano powder, the azodiisobutyronitrile and the 1, 4-dioxane is 1:0.6:0.03: 20.
Example 3
A manufacturing method of a high-frequency mixed compression 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 two surfaces of the substrate by a method combining deposition and electroplating, and etching the surfaces of the two copper plating layers to form a circuit pattern, thus obtaining 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 0.08mm 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, laying a lower circuit board on a flat desktop, and then sequentially laying a first prepreg, a high-frequency material layer, a second prepreg and an upper circuit board on the surface of the lower circuit board according to the sequence to obtain a board to be pressed;
step 4, carrying out hot pressing treatment on the plate to be pressed by using a hydraulic press, specifically: heating the first section of the hydraulic press to 140 ℃, and carrying out heat preservation treatment for 1h under normal pressure; then the temperature is raised to 180 ℃ in the second stage, and the heat preservation treatment is carried out for 0.8h under the condition that the pressure is 1 MPa; then, the temperature is raised to 250 ℃ in the third section, and the heat preservation treatment is carried out for 5 hours under the condition that the pressure is 8 MPa; and finally, reducing the temperature to room temperature under normal pressure to obtain the high-frequency mixing plate.
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 a nickel ditelluride/cage type polysilsesquioxane copolymer and hydrocarbon resin.
The preparation process of the modified hydrocarbon resin comprises the following steps:
dispersing the 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 to the polybutadiene to the N, N-dimethylformamide is 1:25: 20.
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 vinyl trimethoxy silane into an ethanol aqueous solution, and performing ultrasonic dispersion uniformly to obtain a 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 trimethoxy silane to the ethanol aqueous solution is 1:5: 20;
s2, pouring the mixed liquid of the nickel ditelluride into a reflux condensing device, starting stirring, dropwise adding ammonia water with the mass fraction of 15-20% into the mixed liquid of the nickel ditelluride, after dropwise adding, heating to 45-55 ℃, continuously stirring for 8-10 h, cooling, filtering and drying to obtain vinyl nickel ditelluride nanopowder; wherein the mass ratio of the ammonia water to the mixed liquid of the nickel ditelluride is 1: 10;
s2, weighing octavinyl-POSS and 1, 4-dioxane, mixing, adding vinyl ditelluride nano powder after fully mixing, fully mixing again, adding azodiisobutyronitrile, heating to 45-65 ℃, stirring for reacting for 6-8 h, cooling to room temperature, filtering, washing the obtained solid with methanol for three times, and drying to obtain a nickel ditelluride/cage polysilsesquioxane copolymer; wherein the mass ratio of the octavinyl-POSS, the vinyl 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 differs from example 1 in that:
the material of the high-frequency material layer is modified hydrocarbon resin, and the modified hydrocarbon resin is obtained by compounding a nickel ditelluride/cage type 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 nanopowder to the polystyrene to the toluene is 1:22: 15.
Comparative example 2
The high-frequency material layer differs from example 1 in that: the material of the high-frequency material layer is polystyrene.
For more clearly illustrating the invention, the high-frequency material layers prepared in examples 1 to 3 and comparative examples 1 to 2 of the invention were tested and compared in terms of performance, wherein the peel strength was tested according to the method 2.4.8 in test method specification IPC-TM-650; the dielectric constant is determined according to the test method specification IPC-TM-650, method 2.5.5.9, at 1 GHz; the dielectric loss is measured as the dielectric loss tangent at 1GHz according to test method Specification IPC-TM-650, method 2.5.5.9.
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 the embodiments 1 to 3, the high-frequency material layer prepared by the invention has good performance even if different hydrocarbon resins are selected for modification; as can be seen from the example 1 and the comparative examples 1 to 2, compared with the conventional hydrocarbon resin or the common doped hydrocarbon resin, the high-frequency material layer has better performance and is more suitable for being used as a high-frequency material layer.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is 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 on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The manufacturing method of the high-frequency mixed compression plate is characterized by comprising the following steps of:
step 1, cleaning and drying a substrate, cutting the substrate into a proper shape, forming copper plating layers on two surfaces of the substrate, and etching the surfaces of the two copper plating layers to form a circuit pattern, so as to obtain a circuit board;
step 2, preparing two circuit boards obtained 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, laying a lower circuit board on a flat desktop, and then sequentially laying a first prepreg, a high-frequency material layer, a second prepreg and an upper circuit board on the surface of the lower circuit board according to the sequence to obtain a board to be pressed;
and 4, carrying out hot pressing treatment on the plate to be pressed by using a hydraulic machine to obtain the high-frequency mixed plate.
2. The method as claimed in claim 1, wherein in step 1, the substrate is made of ceramic, and the thickness of the substrate is 0.35-0.55 mm.
3. The method as claimed in claim 1, wherein in step 1, the copper plating layer is formed on the surface of the substrate by a combination of deposition and electroplating, and the thickness of each copper plating layer is 0.035-0.05 mm.
4. The method as claimed in claim 1, wherein in step 2, the two prepregs have the same size, material and shape.
5. The method as claimed in claim 1, wherein in step 2, the material of the high-frequency material layer is modified hydrocarbon resin, and 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 thickness of each prepreg of the non-flowing PP sheet of the prepreg is 0.05-0.08 mm.
7. The method for manufacturing a high-frequency hybrid board according to claim 1, wherein in the step 4, the hot pressing process comprises: heating the first section of the hydraulic press to 130-140 ℃, and carrying out heat preservation treatment for 0.5-1 h at normal pressure; heating to 150-180 ℃ in the second stage, and carrying out heat preservation treatment for 0.3-0.8 h under the condition that the pressure is 0.5-1 MPa; then, the temperature is raised to 200-250 ℃ in the third section, and the heat preservation treatment is carried out for 2-5 h under the condition that the pressure is 6-8 MPa; and finally, reducing the temperature to room temperature under normal pressure.
8. The method for manufacturing a high-frequency hybrid compression plate according to claim 1, wherein the modified hydrocarbon resin is obtained by compounding a nickel ditelluride/cage polysilsesquioxane copolymer with a hydrocarbon resin.
9. The method for manufacturing a high-frequency hybrid board according to claim 1, wherein the modified hydrocarbon resin is prepared by the following steps:
dispersing the nickel ditelluride/cage polysilsesquioxane copolymer and the 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 to the hydrocarbon resin to the organic solvent is 1: 18-25: 10-20.
10. The method as claimed in claim 1, wherein the hydrocarbon resin comprises one of styrene-butadiene resin, polystyrene, polydicyclopentadiene, and polybutadiene.
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