CN117820944A - Preparation method of parylene film layer for surface coating of electronic circuit module - Google Patents
Preparation method of parylene film layer for surface coating of electronic circuit module Download PDFInfo
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- CN117820944A CN117820944A CN202410245693.4A CN202410245693A CN117820944A CN 117820944 A CN117820944 A CN 117820944A CN 202410245693 A CN202410245693 A CN 202410245693A CN 117820944 A CN117820944 A CN 117820944A
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- 229920000052 poly(p-xylylene) Polymers 0.000 title claims abstract description 76
- 239000011248 coating agent Substances 0.000 title claims abstract description 40
- 238000000576 coating method Methods 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 22
- 125000003396 thiol group Chemical group [H]S* 0.000 claims abstract description 17
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 16
- KLDXJTOLSGUMSJ-JGWLITMVSA-N Isosorbide Chemical compound O[C@@H]1CO[C@@H]2[C@@H](O)CO[C@@H]21 KLDXJTOLSGUMSJ-JGWLITMVSA-N 0.000 claims abstract description 11
- 229960002479 isosorbide Drugs 0.000 claims abstract description 11
- 230000004048 modification Effects 0.000 claims abstract description 10
- 238000012986 modification Methods 0.000 claims abstract description 10
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229960000834 vinyl ether Drugs 0.000 claims abstract description 9
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims abstract description 8
- PMDRJZUQYMFWSP-UHFFFAOYSA-M trimethyl-[(4-methylphenyl)methyl]azanium;chloride Chemical compound [Cl-].CC1=CC=C(C[N+](C)(C)C)C=C1 PMDRJZUQYMFWSP-UHFFFAOYSA-M 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 24
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 18
- 239000002243 precursor Substances 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000002309 gasification Methods 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 12
- 238000000197 pyrolysis Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- -1 diethyl phosphinate ethylene oxide methyl ester Chemical class 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 6
- 239000012065 filter cake Substances 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 5
- PBYPUGWMDPYEAK-UHFFFAOYSA-N 1,4-dichloro-3,6-dimethylidenecyclohexa-1,4-diene Chemical compound ClC=1C(C=C(C(C1)=C)Cl)=C PBYPUGWMDPYEAK-UHFFFAOYSA-N 0.000 abstract description 4
- KZNRNQGTVRTDPN-UHFFFAOYSA-N 2-chloro-1,4-dimethylbenzene Chemical group CC1=CC=C(C)C(Cl)=C1 KZNRNQGTVRTDPN-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000908 ammonium hydroxide Substances 0.000 abstract description 4
- 125000001453 quaternary ammonium group Chemical group 0.000 abstract description 4
- 239000007787 solid Substances 0.000 abstract description 4
- 239000000758 substrate Substances 0.000 abstract description 4
- 238000005336 cracking Methods 0.000 abstract description 3
- 150000003242 quaternary ammonium salts Chemical class 0.000 abstract description 3
- 150000003254 radicals Chemical class 0.000 abstract description 3
- PCGTXZMDZGOMJG-UHFFFAOYSA-N 2,3-diethyloxirane Chemical compound CCC1OC1CC PCGTXZMDZGOMJG-UHFFFAOYSA-N 0.000 abstract description 2
- 238000005985 Hofmann elimination reaction Methods 0.000 abstract description 2
- 238000007259 addition reaction Methods 0.000 abstract description 2
- XKCQASMZNPBLKI-UHFFFAOYSA-N phosphorosooxymethane Chemical compound COP=O XKCQASMZNPBLKI-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 14
- 238000001914 filtration Methods 0.000 description 12
- 239000000853 adhesive Substances 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 5
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- 239000011347 resin Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
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- 150000003863 ammonium salts Chemical group 0.000 description 4
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- 238000011010 flushing procedure Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 4
- 230000001376 precipitating effect Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229920001187 thermosetting polymer Polymers 0.000 description 4
- VGIVLIHKENZQHQ-UHFFFAOYSA-N n,n,n',n'-tetramethylmethanediamine Chemical compound CN(C)CN(C)C VGIVLIHKENZQHQ-UHFFFAOYSA-N 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 229940125904 compound 1 Drugs 0.000 description 2
- 229940125782 compound 2 Drugs 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 239000012634 fragment Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical group O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
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- 229920006254 polymer film Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 230000003075 superhydrophobic effect Effects 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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Abstract
The invention relates to the technical field of parylene films, in particular to a preparation method of a parylene film layer for coating the surface of an electronic circuit module; the invention takes p-methylbenzyl trimethyl ammonium chloride as a raw material; according to the Hofmann elimination method, in an alkaline environment, quaternary ammonium salt firstly generates quaternary ammonium hydroxide, and then two molecules of quaternary ammonium hydroxide are cyclized to form chloro-p-xylene cyclodimer; sublimating chloro-p-xylene ring into gas state, and cracking into active 2, 5-dichloro-p-dimethylene benzene with free radical; in a polymerization chamber, free 2, 5-dichloro-p-dimethylene benzene is deposited and polymerized on the surface of a solid substrate to form a layer of pinhole-free conformal film; plasma modification is carried out in the thioglycollic acid gas atmosphere, and a film layer with sulfhydryl groups is formed; and (3) performing epoxy-mercapto addition reaction on the isosorbide divinyl ether and diethyl ethylene oxide methyl hypophosphite film layer with mercapto groups to obtain the parylene film layer for coating the surface of the electronic circuit module.
Description
Technical Field
The invention relates to the technical field of parylene films, in particular to a preparation method of a parylene film layer for surface coating of an electronic circuit module.
Background
The parylene film has rapid development and wide application in recent years, is developed into a relatively advanced coating material at home and abroad at present, is a polymer, and has the greatest characteristics of no branched chain, high crystallization, super-large molecular weight and fine process, and is prepared by a vacuum vapor deposition polymerization process to form a completely linear high-crystallization material. The monomer generally introduces different groups or side chains on the benzene ring to form a series of different perrelin series products, and different perrelin films have unique advantages.
The Chinese patent application with publication number of CN117088746A provides a preparation method of a parylene series product, which comprises the following steps: s1, reacting a compound 1 and a compound 2 with N, N, N ', N' -tetramethyl diaminomethane to obtain a bisquaternary ammonium salt; s2, carrying out elimination reaction on the biquaternary ammonium salt and a catalyst under an alkaline condition to obtain a perrelin series product with a general formula shown in formula I; the structural formulas of the compound 1, the compound 2 and the double quaternary ammonium salt are respectively shown as formulas II, III and IV: the invention adopts various benzyl halides to react with N, N, N ', N' -tetramethyl diaminomethane to obtain the biquaternary ammonium salt with a connecting arm; under alkaline condition, the biquaternary ammonium salt and the catalyst are eliminated from being degraded in molecules, N, N, N ', N' -tetramethyl diamino methane is released to form a p-quinone dimethane intermediate state, and the two benzene rings pi conjugation of the intermediate state are more prone to face-to-face ring closing reaction, so that the linear polymerization side reaction of the intermediate state in an end-to-end connection manner can be effectively avoided, the reaction yield is greatly improved, and the parylene series products can be efficiently prepared.
The Chinese patent with the publication number of CN114855142B is issued, and the low-surface-energy parylene material and the preparation method thereof are provided, and based on the existing parylene material, the surface energy of the parylene material is reduced while the original excellent physical and chemical properties of the parylene material are maintained, and the surface of the parylene material after coating can reach a super-hydrophobic state by combining a substrate with a micro-nano structure, so that the self-cleaning property under certain specific working conditions is realized. The low surface energy parylene material is formed by chemical vapor deposition of a parylene raw material and a fluorine-containing reagent. The preparation method comprises the following steps: step 1, placing a parylene raw material and a fluorine-containing reagent into an evaporation chamber; step 2, vacuumizing the whole reaction device to ensure that the reaction occurs under the vacuum condition; step 3, firstly raising the temperature of the cracking furnace to 690 ℃ or 650 ℃, and then raising the temperature of the evaporating chamber to 175 ℃; and 4, depositing a film on the substrate in the room temperature chamber after the raw materials react.
Chinese patent application publication No. CN106905813a discloses a parylene coating, and preparation method and application thereof. The coating mainly comprises a thermosetting resin transition layer and a parylene polymer layer, wherein the thermosetting resin transition layer is used as the transition layer for bonding the parylene polymer layer and the base material. And firstly coating a layer of thermosetting resin on the base material, after the reaction curing degree reaches 50%, depositing the parylene at room temperature, and finally drying and curing completely to obtain the parylene protective coating. The invention takes the thermosetting resin containing aromatic as the transition layer, firstly, the interfacial compatibility between metal, plastic, ceramic and the like as the base material and parylene is reduced; secondly, due to the introduction of benzene rings in the resin and the pi-pi accumulation effect formed between benzene rings in the parylene, the combination between the transition layer and the parylene is firmer.
The parylene film prepared by the above patent and the prior art has complex production equipment, harsh conditions and low yield; the adhesive force is poor, the surface of the coating material is easy to crack and peel, and the loss factor is high.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a preparation method of a parylene film layer for coating the surface of an electronic circuit module, which comprises the following operation steps:
a1: the parylene precursor passes through a gasification furnace, a preheating furnace and a pyrolysis furnace, is pyrolyzed, enters a precooler for cooling, enters a polymerization chamber and is condensed on a glass plate;
a2: after film formation, the film is lifted from the glass plate by a tool to prepare a film layer with the thickness of 0.1-3 mu m;
a3: putting the film layer into plasma equipment, performing plasma modification in a thioglycollic acid gas atmosphere with the radio frequency power of 100W-150W and the gas flow of 20-30ml/min for 30-60S to obtain the film layer with sulfhydryl groups;
a4: according to the weight portions, 2 to 5 portions of isosorbide divinyl ether (CAS: 40268 to 97 to 1), 0.02 to 0.5 portion of diethyl phosphinate ethylene oxide methyl ester, 100 to 120 portions of toluene, 15 to 20 portions of film layer with sulfhydryl groups, 2 to 5 portions of triethylamine, and 30 to 40 ℃ are stirred for 100 to 150 minutes, filtered, washed and dried, and the parylene film layer used for coating the surface of an electronic circuit module is obtained.
Further, the temperature of the gasification furnace is controlled to be 120-140 ℃.
Further, the temperature of the preheating furnace is controlled to be 360-400 ℃.
Further, the temperature of the pyrolysis furnace is controlled between 630 and 650 ℃.
Further, the temperature of the precooler is controlled to be 25-35 ℃.
Further, the vacuum degree of the polymerization chamber is minus 0.08 to minus 0.09Mpa, and the temperature is 20 to 25 ℃.
Further, the preparation method of the parylene precursor comprises the following steps:
k1: weighing 80-100 parts of deionized water in parts by weight in a reactor, opening stirring, continuously adding 20-25 parts of NaOH solution and 15-20 parts of p-methylbenzyl trimethyl ammonium chloride, heating to raise the temperature for reaction, cooling to room temperature after the reaction is finished, carrying out suction filtration, washing to be neutral by using deionized water, and carrying out suction drying;
k2: and (3) after the filter cake is dried in vacuum, 50-80 parts of toluene and 20-30 parts of active carbon are mixed and refluxed, the mixture is filtered, the filtrate is cooled to room temperature, crystals are separated out, the mixture is filtered in a pumping way, the mixture is washed by absolute ethyl alcohol, and the mixture is dried in vacuum to obtain the parylene precursor.
Further, the mass concentration of the NaOH solution is 10-20%.
Further, the reaction temperature of K1 is 90-110 ℃ and the reaction time is 8-12h.
Further, the reflux time of K2 is 50-80min.
Reaction mechanism: 1. p-methylbenzyl trimethyl ammonium chloride is taken as a raw material; according to the Hofmann elimination method, in an alkaline environment, quaternary ammonium salt firstly generates quaternary ammonium hydroxide, and then two molecules of quaternary ammonium hydroxide are cyclized to form chloro-p-xylene cyclodimer;
2. sublimating chloro-p-xylene ring into gas state, and cracking into active 2, 5-dichloro-p-dimethylene benzene with free radical;
3. in a polymerization chamber, free 2, 5-dichloro-p-dimethylene benzene is deposited and polymerized on the surface of a solid substrate to form a layer of pinhole-free conformal film;
4. performing plasma modification on the conformal film in a thioglycollic acid gas atmosphere to obtain a film with sulfhydryl groups;
5. and (3) performing epoxy-mercapto addition reaction on the isosorbide divinyl ether and diethyl ethylene oxide methyl hypophosphite film layer with mercapto groups to obtain the parylene film layer for coating the surface of the electronic circuit module.
Compared with the prior art, the invention has the following remarkable effects:
1. the parylene film layer with isosorbide and diethyl hypophosphorous acid functional groups can improve the adhesive force of the film: through the reaction of isosorbide and diethyl hypophosphorous acid functional groups, strong chemical bonds can be formed between the parylene film layer and the surface of the electronic circuit module, so that the adhesive force is improved;
2. the parylene film layer prepared by the method adopts a vapor deposition process, and gaseous monomers are directly polymerized into a solid polymer film on the solid surface after being cracked into free radicals, so that no matter how complex the form is, no hole is left on the surface of a coating material, no dead angle is left;
3. the parylene film layer prepared by the method has a low loss factor and can be applied to the fields of electronic circuit modules and the like.
Detailed Description
In order to further describe the technical means and effects adopted for achieving the intended purpose of the present invention, the following detailed description will explain specific embodiments, features and effects according to the present invention in conjunction with the preferred embodiments.
Example evaluation method:
1. and (3) adhesive force detection: referring to the cross-cut test of GB/T9286-1998 color paint and varnish films, and scoring according to the test result, wherein 90-100 parts indicate that the cut edge is completely smooth, no lattice is dropped, 80-90 parts indicate that a little coating is dropped at the cut intersection, the affected cross-cut area is less than 5%,70-80 parts indicate that the coating is dropped at the cut intersection and/or along the cut edge, the affected cross-cut area is greater than 5%, less than 15%,50-60 parts indicate that the coating is dropped in large fragments partially or fully along the cut edge, and/or partially or fully dropped on different parts of the lattice, the affected cross-cut area is greater than 15%, and less than 35%,40-50 parts indicate that the coating is dropped in large fragments along the cut edge, and the affected cross-cut area is greater than 35% and less than 65%;
2. solvent resistance test: immersing the parylene film in a cyclohexanone solvent at 60 ℃ for 72 hours, and observing the surface condition of the coating;
3. loss factor test: detection is performed with reference to GB/T18258-2000.
Example 1: the preparation method of the parylene film layer for coating the surface of the electronic circuit module comprises the following operation steps:
a1: the parylene precursor passes through a gasification furnace, a preheating furnace and a pyrolysis furnace, is pyrolyzed, enters a precooler for cooling, enters a polymerization chamber and is condensed on a glass plate;
a2: after film formation, the glass plate is lifted by a tool to prepare a film layer with the thickness of 0.1 mu m;
a3: putting the film layer into plasma equipment, performing plasma modification in a thioglycollic acid gas atmosphere with the radio frequency power of 100W and the gas flow of 20ml/min for 30S to obtain the film layer with the sulfhydryl group;
a4: 2g of isosorbide divinyl ether (CAS: 40268-97-1), 0.02g of diethyl phosphinic acid ethylene oxide methyl ester, 100g of toluene, 15g of film layer with sulfhydryl groups, 2g of triethylamine, stirring at 30 ℃ for 100min, filtering, washing and airing to obtain the parylene film layer for coating the surface of the electronic circuit module.
The temperature of the gasification furnace is controlled at 120 ℃.
The temperature of the preheating furnace is controlled at 360 ℃.
The temperature of the pyrolysis furnace is controlled at 630 ℃.
The temperature of the precooler is controlled at 25 ℃.
The vacuum degree of the polymerization chamber is-0.08 Mpa, and the temperature is 20 ℃.
The preparation method of the parylene precursor comprises the following steps:
k1: weighing 80g of deionized water in a reactor, stirring, continuously adding 20g of NaOH solution and 15g of p-methylbenzyl trimethyl ammonium chloride, heating to raise the temperature for reaction, cooling to room temperature after the reaction is finished, filtering, flushing with deionized water to be neutral, and draining;
k2: and (3) after the filter cake is dried in vacuum, mixing and refluxing with 50g of toluene and 20g of active carbon, filtering, cooling the filtrate to room temperature, precipitating crystals, carrying out suction filtration, washing with absolute ethyl alcohol, and drying in vacuum to obtain the parylene precursor.
The mass concentration of the NaOH solution is 10%.
The reaction temperature of K1 is 90 ℃ and the reaction time is 8h.
The reflux time of K2 is 50min.
Example 2: the preparation method of the parylene film layer for coating the surface of the electronic circuit module comprises the following operation steps:
a1: the parylene precursor passes through a gasification furnace, a preheating furnace and a pyrolysis furnace, is pyrolyzed, enters a precooler for cooling, enters a polymerization chamber and is condensed on a glass plate;
a2: after film formation, the film is lifted from the glass plate by a tool to prepare a film layer with the thickness of 1 mu m;
a3: putting the film layer into plasma equipment, performing plasma modification in a thioglycollic acid gas atmosphere with the radio frequency power of 110W and the gas flow of 25ml/min for 40S to obtain the film layer with the sulfhydryl group;
a4: 3g of isosorbide divinyl ether (CAS: 40268-97-1), 0.2g of diethyl phosphinic acid ethylene oxide methyl ester, 105g of toluene, 16g of film layer with sulfhydryl groups, 3g of triethylamine, stirring for 110min at 35 ℃, filtering, washing and airing to obtain the parylene film layer for coating the surface of the electronic circuit module.
The temperature of the gasification furnace is controlled at 125 ℃.
The temperature of the preheating furnace is controlled at 370 ℃.
The temperature of the pyrolysis furnace is controlled at 635 ℃.
The temperature of the precooler is controlled at 30 ℃.
The vacuum degree of the polymerization chamber is-0.08 Mpa, and the temperature is 20 ℃.
The preparation method of the parylene precursor comprises the following steps:
k1: weighing 85g of deionized water in a reactor, stirring, continuously adding 22g of NaOH solution and 16g of p-methylbenzyl trimethyl ammonium chloride, heating to raise the temperature for reaction, cooling to room temperature after the reaction is finished, filtering, flushing with deionized water to be neutral, and draining;
k2: and (3) after the filter cake is dried in vacuum, mixing and refluxing with 60g of toluene and 23g of active carbon, filtering, cooling the filtrate to room temperature, precipitating crystals, carrying out suction filtration, washing with absolute ethyl alcohol, and drying in vacuum to obtain the parylene precursor.
The mass concentration of the NaOH solution is 15%.
The reaction temperature of K1 is 95 ℃ and the reaction time is 9h.
The reflux time of K2 is 60min.
Example 3: the preparation method of the parylene film layer for coating the surface of the electronic circuit module comprises the following operation steps:
a1: the parylene precursor passes through a gasification furnace, a preheating furnace and a pyrolysis furnace, is pyrolyzed, enters a precooler for cooling, enters a polymerization chamber and is condensed on a glass plate;
a2: after film formation, the film is lifted from the glass plate by a tool to prepare a film layer with the thickness of 2 mu m;
a3: putting the film layer into plasma equipment, performing plasma modification in a thioglycollic acid gas atmosphere with the radio frequency power of 140W and the gas flow of 25ml/min for 50S to obtain the film layer with sulfhydryl groups;
a4: 4g of isosorbide divinyl ether (CAS: 40268-97-1), 0.4g of diethyl phosphinic acid ethylene oxide methyl ester, 115g of toluene, 19g of film layer with sulfhydryl groups, 4g of triethylamine, stirring at 35 ℃ for 140min, filtering, washing and airing to obtain the parylene film layer for coating the surface of the electronic circuit module.
The temperature of the gasification furnace is controlled at 135 ℃.
The temperature of the preheating furnace is controlled at 390 ℃.
The temperature of the pyrolysis furnace is controlled at 645 ℃.
The temperature of the precooler is controlled at 30 ℃.
The vacuum degree of the polymerization chamber is-0.09 Mpa, and the temperature is 25 ℃.
The preparation method of the parylene precursor comprises the following steps:
k1: weighing 95g of deionized water in a reactor, stirring, continuously adding 24g of NaOH solution and 18g of p-methylbenzyl trimethyl ammonium chloride, heating to raise the temperature for reaction, cooling to room temperature after the reaction is finished, filtering, flushing with deionized water to be neutral, and draining;
k2: and (3) after the filter cake is dried in vacuum, mixing and refluxing with 70g of toluene and 28g of active carbon, filtering, cooling the filtrate to room temperature, precipitating crystals, carrying out suction filtration, washing with absolute ethyl alcohol, and drying in vacuum to obtain the parylene precursor.
The mass concentration of the NaOH solution is 15%.
The reaction temperature of K1 is 105 ℃, and the reaction time is 11h.
The reflux time of K2 is 70min.
Example 4: the preparation method of the parylene film layer for coating the surface of the electronic circuit module comprises the following operation steps:
a1: the parylene precursor passes through a gasification furnace, a preheating furnace and a pyrolysis furnace, is pyrolyzed, enters a precooler for cooling, enters a polymerization chamber and is condensed on a glass plate;
a2: after film formation, the glass plate is lifted by a tool to prepare a film layer with the thickness of 3 mu m;
a3: putting the film layer into plasma equipment, performing plasma modification in a thioglycollic acid gas atmosphere with the radio frequency power of 150W, and the gas flow rate of 30ml/min and the treatment time of 60S to obtain the film layer with sulfhydryl groups;
a4: 5g of isosorbide divinyl ether (CAS: 40268-97-1), 0.5g of diethyl phosphinic acid ethylene oxide methyl ester, 120 g toluene, 20g film layers with sulfhydryl groups, 5g of triethylamine, stirring at 40 ℃ for 150min, filtering, washing and airing to obtain the parylene film layer for coating the surface of the electronic circuit module.
The temperature of the gasification furnace is controlled at 140 ℃.
The temperature of the preheating furnace is controlled at 400 ℃.
The temperature of the pyrolysis furnace is controlled at 650 ℃.
The temperature of the precooler is controlled at 35 ℃.
The vacuum degree of the polymerization chamber is-0.09 Mpa, and the temperature is 25 ℃.
The preparation method of the parylene precursor comprises the following steps:
k1: weighing 100g of deionized water in a reactor, stirring, continuously adding 25g of NaOH solution and 20g of p-methylbenzyl trimethyl ammonium chloride, heating to raise the temperature for reaction, cooling to room temperature after the reaction is finished, filtering, flushing with deionized water to be neutral, and draining;
k2: and (3) after the filter cake is dried in vacuum, mixing and refluxing with 80g of toluene and 30g of active carbon, filtering, cooling the filtrate to room temperature, precipitating crystals, carrying out suction filtration, washing with absolute ethyl alcohol, and drying in vacuum to obtain the parylene precursor.
The mass concentration of the NaOH solution is 20%.
The reaction temperature of K1 is 110 ℃, and the reaction time is 12h.
The reflux time of K2 is 80min.
Comparative example 1: in this example, isosorbide divinyl ether was not added during the preparation of the parylene film layer, and the procedure of example 1 was followed.
Comparative example 2: in this example, diethyl phosphinate ethylene oxide methyl ester was not added during the preparation of the parylene film, otherwise the same as in example 1.
Comparative example 3: in this example, a film layer with mercapto group was not added in the preparation process of the parylene film layer, and the same procedure as in example 1 was followed.
Table 1: test results for each example and comparative example
Through data analysis of each example and comparative example in table 1, the parylene film prepared by the invention has good adhesive force; the surface of the coating material is intact; the low-loss-factor circuit has a low loss factor and can be applied to the fields of electronic circuit modules and the like.
The present invention is not limited to the above embodiments, but is capable of modification and variation in detail, and other modifications and variations can be made by those skilled in the art without departing from the scope of the present invention.
Claims (10)
1. The preparation method of the parylene film layer for coating the surface of the electronic circuit module is characterized by comprising the following steps of: the operation steps are as follows:
a1: the parylene precursor passes through a gasification furnace, a preheating furnace and a pyrolysis furnace, is pyrolyzed, enters a precooler for cooling, enters a polymerization chamber and is condensed on a glass plate;
a2: after film formation, the film is lifted from the glass plate by a tool to prepare a film layer with the thickness of 0.1-3 mu m;
a3: putting the film layer into plasma equipment, performing plasma modification in a thioglycollic acid gas atmosphere with the radio frequency power of 100W-150W and the gas flow of 20-30ml/min for 30-60S to obtain the film layer with sulfhydryl groups;
a4: according to the weight portions, 2 to 5 portions of isosorbide divinyl ether, 0.02 to 0.5 portion of diethyl phosphinate ethylene oxide methyl ester, 100 to 120 portions of toluene, 15 to 20 portions of film layer with sulfhydryl groups, 2 to 5 portions of triethylamine and 30 to 40 ℃ are stirred for 100 to 150 minutes, filtered, washed and dried to obtain the parylene film layer for coating the surface of the electronic circuit module.
2. The method for preparing a parylene film layer for surface coating of an electronic circuit module according to claim 1, wherein the method comprises the following steps: the temperature of the gasification furnace is controlled between 120 and 140 ℃.
3. The method for preparing a parylene film layer for surface coating of an electronic circuit module according to claim 1, wherein the method comprises the following steps: the temperature of the preheating furnace is controlled between 360 and 400 ℃.
4. The method for preparing a parylene film layer for surface coating of an electronic circuit module according to claim 1, wherein the method comprises the following steps: the temperature of the pyrolysis furnace is controlled between 630 and 650 ℃.
5. The method for preparing a parylene film layer for surface coating of an electronic circuit module according to claim 1, wherein the method comprises the following steps: the temperature of the precooler is controlled to be 25-35 ℃.
6. The method for preparing a parylene film layer for surface coating of an electronic circuit module according to claim 1, wherein the method comprises the following steps: the vacuum degree of the polymerization chamber is-0.08 to-0.09 Mpa, and the temperature is 20-25 ℃.
7. The method for preparing a parylene film layer for surface coating of an electronic circuit module according to claim 1, wherein the method comprises the following steps: the preparation method of the parylene precursor comprises the following steps:
k1: weighing 80-100 parts of deionized water in parts by weight in a reactor, opening stirring, continuously adding 20-25 parts of NaOH solution and 15-20 parts of p-methylbenzyl trimethyl ammonium chloride, heating to raise the temperature for reaction, cooling to room temperature after the reaction is finished, carrying out suction filtration, washing to be neutral by using deionized water, and carrying out suction drying;
k2: and (3) after the filter cake is dried in vacuum, 50-80 parts of toluene and 20-30 parts of active carbon are mixed and refluxed, the mixture is filtered, the filtrate is cooled to room temperature, crystals are separated out, the mixture is filtered in a pumping way, the mixture is washed by absolute ethyl alcohol, and the mixture is dried in vacuum to obtain the parylene precursor.
8. The method for preparing a parylene film layer for surface coating of an electronic circuit module according to claim 7, wherein: the mass concentration of the NaOH solution is 10-20%.
9. The method for preparing a parylene film layer for surface coating of an electronic circuit module according to claim 7, wherein: the reaction temperature of K1 is 90-110 ℃ and the reaction time is 8-12h.
10. The method for preparing a parylene film layer for surface coating of an electronic circuit module according to claim 7, wherein: the reflux time of K2 is 50-80min.
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