CN114245613A - Carbon black pore solution, preparation method thereof and black pore process - Google Patents
Carbon black pore solution, preparation method thereof and black pore process Download PDFInfo
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- CN114245613A CN114245613A CN202111448725.3A CN202111448725A CN114245613A CN 114245613 A CN114245613 A CN 114245613A CN 202111448725 A CN202111448725 A CN 202111448725A CN 114245613 A CN114245613 A CN 114245613A
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- carbon black
- pore
- black
- hole
- pore liquid
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- 239000006229 carbon black Substances 0.000 title claims abstract description 81
- 239000011148 porous material Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 40
- 230000008569 process Effects 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 45
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 15
- 239000002562 thickening agent Substances 0.000 claims description 15
- 238000000926 separation method Methods 0.000 claims description 13
- 239000003995 emulsifying agent Substances 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 239000003945 anionic surfactant Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000010008 shearing Methods 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000005530 etching Methods 0.000 claims description 8
- 230000000844 anti-bacterial effect Effects 0.000 claims description 7
- 239000003899 bactericide agent Substances 0.000 claims description 7
- -1 benzyl alcohol, dodecyl alcohol ester Chemical class 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000002736 nonionic surfactant Substances 0.000 claims description 5
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 5
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims description 4
- IBLKWZIFZMJLFL-UHFFFAOYSA-N 1-phenoxypropan-2-ol Chemical compound CC(O)COC1=CC=CC=C1 IBLKWZIFZMJLFL-UHFFFAOYSA-N 0.000 claims description 4
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
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- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- LQZZUXJYWNFBMV-UHFFFAOYSA-N ethyl butylhexanol Natural products CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
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- 238000007654 immersion Methods 0.000 claims description 3
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- 229920005989 resin Polymers 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- JIHQDMXYYFUGFV-UHFFFAOYSA-N 1,3,5-triazine Chemical class C1=NC=NC=N1 JIHQDMXYYFUGFV-UHFFFAOYSA-N 0.000 claims description 2
- RWNUSVWFHDHRCJ-UHFFFAOYSA-N 1-butoxypropan-2-ol Chemical compound CCCCOCC(C)O RWNUSVWFHDHRCJ-UHFFFAOYSA-N 0.000 claims description 2
- JOLQKTGDSGKSKJ-UHFFFAOYSA-N 1-ethoxypropan-2-ol Chemical compound CCOCC(C)O JOLQKTGDSGKSKJ-UHFFFAOYSA-N 0.000 claims description 2
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 2
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 2
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 2
- 229960001631 carbomer Drugs 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 150000007942 carboxylates Chemical class 0.000 claims description 2
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- 235000019438 castor oil Nutrition 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 239000010696 ester oil Substances 0.000 claims description 2
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- 239000000194 fatty acid Substances 0.000 claims description 2
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- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 2
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 2
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 2
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 2
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 2
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- MGIYRDNGCNKGJU-UHFFFAOYSA-N isothiazolinone Chemical compound O=C1C=CSN1 MGIYRDNGCNKGJU-UHFFFAOYSA-N 0.000 claims description 2
- 229920000609 methyl cellulose Polymers 0.000 claims description 2
- 239000001923 methylcellulose Substances 0.000 claims description 2
- 235000010981 methylcellulose Nutrition 0.000 claims description 2
- 230000003472 neutralizing effect Effects 0.000 claims description 2
- 239000003002 pH adjusting agent Substances 0.000 claims description 2
- 229920000058 polyacrylate Polymers 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 2
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 2
- 239000011736 potassium bicarbonate Substances 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 235000011181 potassium carbonates Nutrition 0.000 claims description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 2
- 239000000661 sodium alginate Substances 0.000 claims description 2
- 235000010413 sodium alginate Nutrition 0.000 claims description 2
- 229940005550 sodium alginate Drugs 0.000 claims description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 2
- 238000009713 electroplating Methods 0.000 abstract description 16
- 230000007547 defect Effects 0.000 abstract description 8
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 36
- 229910052802 copper Inorganic materials 0.000 description 35
- 239000010949 copper Substances 0.000 description 35
- 230000000052 comparative effect Effects 0.000 description 28
- 238000012360 testing method Methods 0.000 description 26
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- 239000000203 mixture Substances 0.000 description 14
- 238000004061 bleaching Methods 0.000 description 6
- 238000007747 plating Methods 0.000 description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 4
- 238000001465 metallisation Methods 0.000 description 4
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- 239000000126 substance Substances 0.000 description 4
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- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- DYUQAZSOFZSPHD-UHFFFAOYSA-N Phenylpropanol Chemical group CCC(O)C1=CC=CC=C1 DYUQAZSOFZSPHD-UHFFFAOYSA-N 0.000 description 2
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- DEXFNLNNUZKHNO-UHFFFAOYSA-N 6-[3-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperidin-1-yl]-3-oxopropyl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1CCN(CC1)C(CCC1=CC2=C(NC(O2)=O)C=C1)=O DEXFNLNNUZKHNO-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
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- 239000002131 composite material Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
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- 230000001737 promoting effect Effects 0.000 description 1
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- 229920003031 santoprene Polymers 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
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Images
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
- H05K3/40—Forming printed elements for providing electric connections to or between printed circuits
- H05K3/42—Plated through-holes or plated via connections
- H05K3/423—Plated through-holes or plated via connections characterised by electroplating method
- H05K3/424—Plated through-holes or plated via connections characterised by electroplating method by direct electroplating
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
-
- 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
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
- H05K2203/07—Treatments involving liquids, e.g. plating, rinsing
- H05K2203/0779—Treatments involving liquids, e.g. plating, rinsing characterised by the specific liquids involved
Abstract
The invention provides a carbon black pore liquid, a preparation method thereof and a black pore process. The PCB/FPC surface after the carbon black hole liquid black hole treatment of the invention is clean without residual carbon, the surface after electroplating is smooth, and the defects are obviously reduced.
Description
Technical Field
The invention relates to the technical field of circuit board manufacturing, in particular to a carbon black pore solution, a preparation method thereof and a black pore process.
Background
After the PCB/FPC is drilled by mechanical or laser, because the middle area of the circuit board is an insulating non-conducting part, conductive connection is needed among all layers for realizing the functions of the product, the hole needs to be electroplated with copper, and the precondition for the electroplated copper treatment is that the insulating state of the hole wall needs to be eliminated and the hole wall is changed into a conductive state. The first approach was to use micro-rivets, which severely limited the high reliability, versatility and precision of the circuit boards, and the chemical copper deposition (PTH) process was later developed. For some time, chemical copper deposition (PTH) has been used. But the PTH solution contains various chemical substances which are harmful to the ecological environment, such as EDTA, NTA, EDTP and formaldehyde which is easy to cause cancer, and the wastewater treatment is complex and the cost is high. In addition, the stability of the PTH solution is poor, and the analysis and maintenance of the solution are complicated. Meanwhile, the PTH copper plating layer has poor mechanical properties and a complicated process flow. Therefore, the industry is always searching for new hole metallization technology, and the black hole direct plating technology is produced under the background.
At present, black hole liquid adopted by black hole treatment is mainly monopolized by foreign manufacturers. With the aggravation of international trade disputes in recent years, the domestic circuit board industry is restricted by foreign material suppliers and has low cost requirements, and a high-stability black hole liquid which is independently researched and developed is urgently needed.
Disclosure of Invention
Therefore, the carbon black pore solution, the preparation method thereof and the black pore process are needed to be provided, the stability is high, and the black pore process performance requirement in the production of the circuit board can be met.
The invention adopts the following technical scheme:
the invention provides a carbon black pore liquid which is a suspension liquid with a pH value of 9.8-10.6, and is prepared by mixing the following raw materials in percentage by weight: 2 to 10 percent of nano-scale carbon black, 0.05 to 2 percent of thickening agent, 0.1 to 2 percent of film forming agent, 1 to 5 percent of emulsifying agent, 0.5 to 2 percent of acid-base regulator, 0.05 to 1.5 percent of bactericide and the balance of water; wherein the film forming agent is selected from at least one of benzyl alcohol, dodecyl alcohol ester, ethylene glycol butyl ether, propylene glycol methyl ether, propylene glycol ethyl ether, propylene glycol butyl ether and propylene glycol phenyl ether, and the emulsifier is selected from anionic surfactant or nonionic surfactant; the preparation method of the nano-scale carbon black comprises the following steps: adding 98% concentrated sulfuric acid into carbon black prepared by a gas black method according to the volume ratio of (1-2):1, stirring and soaking for 2-3h, then adding deionized water for dilution, removing acid liquor, then adding ammonia water for neutralizing residual acid liquor until the pH value is more than 7, carrying out centrifugal separation, then carrying out deionized water immersion cleaning and centrifugal separation for 5-6 times, and when the pH value is detected to be 7-9, drying and dehydrating and grinding until the average particle size is not more than 200nm to obtain carbon black powder; removing impurity iron from the carbon black powder to obtain the nano-scale carbon black.
Preferably, the carbon black pore solution is a suspension with a pH value of 9.8-10.6 prepared by mixing the following raw materials in percentage by weight: 2 to 4 percent of nano-scale carbon black, 0.05 to 2 percent of thickening agent, 0.1 to 1 percent of film forming agent, 1 to 2 percent of emulsifying agent, 0.5 to 2 percent of acid-base regulator, 0.05 to 0.5 percent of bactericide and the balance of water.
In some of these embodiments, the thickening agent is selected from at least one of methylcellulose, hydroxyethylcellulose, hydroxypropylmethylcellulose, sodium carboxymethylcellulose, polyvinyl alcohol, sodium alginate polyacrylate, polyacrylamide, polyvinylpyrrolidone, polyethylene oxide, carbomer resin, polyacrylic acid.
In some of these embodiments, the pH adjusting agent is selected from at least one of potassium carbonate, sodium bicarbonate, potassium bicarbonate, ammonia, ethanolamine.
In some of these embodiments, the emulsifier is selected from at least one of a sulfate type anionic surfactant, a sulfonate type anionic surfactant, and a carboxylate type anionic surfactant.
In some of the embodiments, the nonionic surfactant is selected from at least one of fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, fatty acid polyoxyethylene ester, and castor oil polyoxyethylene ether.
In some of these embodiments, the biocide is selected from at least one of s-triazine, isothiazolinone biocides.
The invention also provides a preparation method of the carbon black pore solution, which comprises the following steps: respectively preparing a film forming agent aqueous solution and a thickening agent aqueous solution, uniformly mixing the film forming agent aqueous solution and the thickening agent aqueous solution, and adding the rest water to form an intermediate mixed solution; adding an emulsifier and an acid-base regulator into the intermediate mixed solution, uniformly stirring, adding nano-scale carbon black, shearing, stirring and dispersing to form a suspension; grinding the suspension, and controlling the particle size range to be 140-180nm to obtain the material.
In some of these embodiments, the process parameters of the shear agitation are: the rotating speed is not lower than 2000r/min, and the shearing dispersion time is not lower than 2 h.
The invention also provides a black hole processing technology, which comprises the following steps: providing a sample plate to be subjected to black hole treatment, matching with microetching, cleaning, washing, hole finishing and plate drying processes, and treating by using the carbon black hole liquid to obtain a sample piece to be plated with copper.
Compared with the prior art.
The carbon black pore liquid is compounded by nano-scale carbon black, a thickening agent, a specific type of film forming agent, a specific type of emulsifying agent, an acid-base regulator, a bactericide and water according to a specific proportion, and the whole carbon black pore liquid has high particle size stability. The PCB/FPC surface treated by the carbon black hole liquid black hole treatment of the invention is clean without carbon residue, the electroplated surface is smooth without surface defects caused by carbon residue visible to naked eyes, the abnormal defect of hole copper separation of triple tin bleaching (288 ℃) after the hole plate is electroplated with copper is obviously reduced, and the abnormal defect of hole copper separation of secondary tin bleaching (288 ℃) of the slot plate is obviously reduced.
Drawings
FIG. 1 is a schematic diagram of a specimen structure for an electroplating speed test.
FIG. 2 is a schematic view of a test strip for defect testing of copper-free holes.
FIG. 3 is a schematic structural diagram of a sample wafer for a hot tin-bleaching test.
Fig. 4 is a schematic view of a partial structure of a ten-thousand-hole plate.
FIG. 5 is a diagram illustrating a TP calculation method.
Detailed Description
The present invention is further described in detail below with reference to specific examples so that those skilled in the art can more clearly understand the present invention.
The following examples are provided only for illustrating the present invention and are not intended to limit the scope of the present invention. All other embodiments obtained by a person skilled in the art based on the specific embodiments of the present invention without any inventive step are within the scope of the present invention.
In the examples of the present invention, all the raw material components are commercially available products well known to those skilled in the art, unless otherwise specified; in the examples of the present invention, unless otherwise specified, all technical means used are conventional means well known to those skilled in the art.
The key raw material sources are as follows:
dodecanol ester, available from bioscience, GmbH, Yibang, GmbH.
Propylene glycol phenyl ether, sample dow, usa.
Polyacrylamide, available from santoprene, ltd.
Polyvinyl alcohol, available from Shandong Xiang Showa New materials Co.
Example 1
The embodiment provides a carbon black pore liquid, the pH value of which is 9.8-10.6, and the raw material composition of which is shown in the following table 1:
table 1 carbon black pore liquid raw material composition of example 1
The preparation method of the carbon black pore liquid comprises the following steps:
s1, preparing nano carbon black:
carbon black obtained by the gas black process (hydrocarbon combustion) is subjected to oxidation treatment and purification.
Wherein, the oxidation treatment adopts a concentrated sulfuric acid soaking method: mixing carbon black to be treated in a volume ratio of 1-2: adding 98% concentrated sulfuric acid into 1, stirring and soaking for 2-3h, then adding deionized water with the volume 2 times that of the concentrated sulfuric acid for dilution, removing acid liquor in a centrifugal separation mode, adding ammonia water into the carbon black to neutralize residual acid liquor until the pH value is greater than 7, carrying out centrifugal separation, then carrying out deionized water immersion cleaning and centrifugal separation for 5-6 times, and when the pH value is detected to be 7-9, drying, dehydrating and grinding until the average particle size is not greater than 200nm to obtain carbon black powder.
Wherein, the purification treatment can be any one of an acid-base method, a hydrofluoric acid method, a flotation method, a magnetic separation method or a high-temperature purification method. In the embodiment, the purification treatment is preferably a magnetic separation method, wherein the carbon black powder after the oxidation treatment passes through a magnetic (magnetic field strength is 1000-.
S2, adding the film forming agent into deionized water according to the weight ratio of the raw materials to water of 1:5, heating to 75 +/-5 ℃, stirring for 2-4 hours to dissolve the film forming agent, and filtering the film forming agent which is not completely dissolved by a stainless steel filter screen with the aperture of 0.2mm for later use to obtain a film forming agent solution. Adding the thickening agent into deionized water according to the weight ratio of the thickening agent to water being 1 (20-25), standing for 10-15h, and filtering the thickening agent which is not completely dissolved by using a stainless steel filter screen with the aperture of 0.2mm for later use after the thickening agent is completely dissolved.
S3, mixing the film forming agent and the thickening agent, adding the balance of deionized water, adding the emulsifier, the pH regulator and the bactericide in proportion, uniformly stirring, and finally adding the nano-scale carbon black into the mixing system, wherein the carbon black needs to be added in a high-speed shearing and dispersing reaction kettle with the rotating speed of not less than 2000 rpm. The high-speed shearing dispersion time is not less than 2 hours, and the shearing suspension is obtained.
And S4, transferring the sheared suspension into a grinding machine for grinding, wherein the grinding time is set to be 8-12 hours, the particle size needs to be detected by a laser particle size scatterometer after grinding, and the particle size range needs to be controlled to be 140-180 nm.
Example 2
The embodiment provides a carbon black pore liquid, the pH value of which is 9.8-10.6, and the raw material composition of which is shown in the following table 2:
table 2 carbon black pore liquid raw material composition of example 2
The preparation method of the black hole liquid of the embodiment is basically the same as that of the embodiment 1.
Example 3
The embodiment provides a carbon black pore liquid, the pH value of which is 9.8-10.6, and the raw material composition of which is shown in table 3 below:
table 3 carbon black pore liquid feedstock composition of example 3
The preparation method of the carbon black pore solution in the embodiment is basically the same as that of the embodiment 1.
Example 4
The embodiment provides a carbon black pore liquid, the pH value of which is 9.8-10.6, and the raw material composition of which is shown in the following table 4:
table 4 carbon black pore liquid feedstock composition of example 4
The preparation method of the carbon black pore solution in the embodiment is basically the same as that of the embodiment 1.
Comparative example 1
This comparative example provides a carbon black bore fluid having a pH of 9.8 to 10.6 and the same raw material composition as in example 1, except that: the content of the nano-scale carbon black is 12 wt%, the nano-scale carbon black does not contain sodium dodecyl sulfate, and only contains 1.2 wt% of alkylphenol polyoxyethylene OP-9.
The preparation method of the carbon black pore solution of the comparative example is basically the same as that of example 1.
Comparative example 2
This comparative example provides a carbon black bore fluid having a pH of 9.8 to 10.6 and a raw material composition as shown in Table 5 below:
table 5 composition of black pore liquid raw material of comparative example 2
The comparative example black pore liquid was prepared in substantially the same manner as in example 1.
Comparative example 3
This comparative example provides a carbon black bore fluid having substantially the same composition as example 1, except that: does not contain film forming agent.
Comparative example 4
This comparative example provides a carbon black bore fluid having substantially the same composition as example 1, except that: the film forming agent is phenylpropanol.
Performance detection
1) The carbon black pore liquids prepared in examples 1 to 4 and comparative examples 1 to 4 were subjected to particle size tests, respectively. The results of the test by the Malvern laser particle size tester are shown in the following table:
2) black hole treatment
The metallization process flow of the black holes is as follows:
micro etching → water washing → black hole → dry plate combination → whole hole → water washing → black hole → dry plate combination → micro etching → dry plate combination.
The specific process parameters are shown in the following table:
remarks explanation:
(1) cleaning and hole preparation
Cleaning and pore-forming are respectively carried out by using cleaning agent GZ-1701 and pore-forming agent GZ-1702. GZ-1701 and whole pore agent GZ-1702 are cleaning and regulating agents before black pore formation for direct electroplating of the microporous circuit board. GZ-1701 and GZ-1702 are alkaline, contain a small amount of composite additives, and mainly have the functions of adjusting the original negative charges on the surfaces of the glass fibers and the resin into positive charges and promoting the adsorption of the negatively charged particles in the black pore liquid.
(2) The conventional black hole solution GZ-1703 is an alkaline solution containing carbon black suspended particles and a surfactant, the pH value is 9.8-10.6, and a continuous conductive carbon black film is provided in a hole of a circuit board so as to facilitate subsequent copper electroplating.
(3) And (3) a dry plate combination process:
the method mainly has the functions of removing more than 90 percent of water in the carbon black layer uniformly distributed on the hole wall and the copper surface, wherein the temperature is 60-85 ℃, the time is about 55 seconds, and the method is provided with an air knife and the pressure is 1000 mmAq; if the temperature is too low, the moisture in the small holes or the deep holes is not easy to dry, and the carbon black layer is easy to wash away in the subsequent micro-etching section.
(4) Micro etching
The micro-etching liquid is used for removing carbon black on the surface copper foil and the inner layer copper of the hole wall and carrying out micro-etching on the copper surface so as to provide a micro-rough surface for facilitating the subsequent electro-coppering process. The materials required by the process are SPS and H2SO4、CuSO4。
As shown in FIG. 1, the plating rate test was carried out using a standard test piece for a black hole process: the standard test piece simulates the field process condition treatment, and other procedures are the same except that the black hole liquid of different test examples is different. Then, a Hull cell was used for electroplating (unified bath) simulation, and the electroplating conditions were as follows: the current is 1 ampere, the electroplating time is 10min, and the temperature is normal temperature.
The pore climbing test results are statistically shown in the following table:
| carbon black pore liquid used in test examples | Result of hole climbing |
| Example 1 | High 6 low 6 |
| Example 2 | High 7 low 6 |
| Example 3 | High 7 low 5 |
| Example 4 | High 7 low 5 |
| Comparative example 1 | High 5 low 3 |
| Comparative example 2 | |
| Comparative example 3 | High 5 low 3 |
| Comparative example 4 | |
Remarks explanation: the left side of the test piece is a high current area (high area or high area for short), the right side of the test piece is a low current area (low area or low for short), the following numbers indicate the number of the conducted holes, the larger the number, the better the effect, and the minimum standard is 5 higher than 4 lower.
Defect test for investigating whether holes have copper or not
The test method comprises the following steps: taking 8 test pieces (the number of drilled holes is 65000+), simulating an on-site process to carry out unified treatment (only carbon black pore liquid is different), and the rest are the same. After treatment, VCP electroplating is carried out in a certain customer factory, and the electroplating quality of the plate surface is inspected completely (whether holes appear or not without copper) visually. The test results are as follows:
| black hole liquid used in test examples | Plate surface inspection results (the less the hole has no copper, the better) |
| Example 1 | No copper in the 0 hole |
| Example 2 | No copper in the 0 hole |
| Example 3 | 1 hole has no copper |
| Example 4 | No copper in the 0 hole |
| Comparative example 1 | 3 holes without copper |
| Comparative example 2 | 5 holes without copper |
| Comparative example 3 | 5 holes without copper |
| Comparative example 4 | 7 holes have no copper |
Hot tin-bleaching test for inspecting whether pore copper separation occurs
The test method comprises the following steps: taking 3 test pieces of each test respectively, slicing to detect whether hole copper separation occurs, wherein the statistical results are shown in the following table:
| black hole liquid used in test examples | Number of copper holes (the smaller the number, the better) |
| Example 1 | 0 |
| Example 2 | 0 |
| Example 3 | 1 |
| Example 4 | 0 |
| Comparative example 1 | 4 |
| Comparative example 2 | 3 |
| Comparative example 3 | 4 |
| Comparative example 4 | 6 |
Universal orifice plate test
The test method comprises the following steps: selecting a circuit board with the number of micropores exceeding 10000, simulating field process (only carbon black pore liquid is different), then carrying out whole procedures of electroplating, patterning, developing, etching and the like, and testing the resistance between the initial two pores of the ten-thousand pore plate of the well-made circuit by using a universal meter.
TP value test
As shown in fig. 5, the experimental method includes the following steps: the method comprises the following steps of taking 8 scrapped FPC products (without affecting black holes and electroplating) of a certain customer with the same specification, processing the scrapped FPC products by different black hole solutions, passing through the same VCP electroplating line, cutting out a part of the VCP electroplating line to be sliced, observing and measuring by using an optical microscope to calculate, and obtaining a statistical result shown in the following table:
| black hole liquid used in test examples | Throwing power TP value (%) (the larger the better) |
| Example 1 | 154 |
| Example 2 | 152 |
| Example 3 | 157 |
| Example 4 | 148 |
| Comparative example 1 | 124 |
| Comparative example 2 | 118 |
| Comparative example 3 | 116 |
| Comparative example 4 | 112 |
Remarking: generally, more than 120% of the total amount of the composition is regarded as acceptable.
As can be seen from the above table: the carbon black pore liquid of the embodiments 1 to 4 can meet the requirement of direct electroplating of a circuit board, the quality and the performance of the carbon black pore liquid reach or exceed the traditional copper deposition PTH and polymer conductive film process, and the carbon black pore liquid can be widely applied to the hole metallization process of the circuit board.
In addition, it is worth to be noted that, after a great deal of research, the inventor team found that: when the content of the nano-scale carbon black in the black hole liquid is 2-10%, the content of the thickening agent is 0.05-2%, the content of the film forming agent is 0.1-2%, the content of the emulsifying agent is 1-5%, the content of the alkaline regulator is 0.5-2%, and the content of the bactericide is 0.05-1.5%, the film forming agent is preferably selected from propylene glycol phenyl ether and/or dodecyl alcohol ester, and the emulsifying agent is selected from anionic surfactants or nonionic surfactants, so that the performance requirements of high hole climbing speed, low hole breaking rate, excellent hole copper binding force and high deep plating capacity TP value can be integrally met in the production and application of circuit boards:
1) the suspension is dispersed by high-speed shearing, the system stability is superior to similar products on the market, and the stable production and operation can be carried out for 12-18 months by market verification, and the particle size of the carbon black can still be stabilized below 400 nanometers.
2) Because the control range of the carbon black particle diameter is narrow, the PCB/FPC surface after the carbon black hole metallization treatment of the company is clean and has no residual carbon residue, the surface after the electroplating is flat, and no surface defect caused by the residual carbon can be seen by naked eyes.
3) The special film forming additive of the product promotes carbon black to form a complete conductive film, and can effectively reduce the abnormal defects of no copper in PCB/FPC holes, three-time tin bleaching (288 ℃) hole copper separation after the copper is electroplated on the hole plate and two-time tin bleaching (288 ℃) hole copper separation on the slot hole plate.
4) The electroplating deep plating capacity (TP value, the TP value is equal to the thickness of the thinnest copper of the hole wall/the average copper thickness of the surface X100 percent) is more than 100 percent in the whole life cycle (12 months) of the black hole liquid, and the resistance of a ten thousand hole plates (the number of drilled holes on the plates is more than 10000) is less than 45 ohm.
5) When the film forming agent is phenylpropanol or other substances, the stability of the carbon black pore solution is reduced, and the pore breaking rate is increased in the later period of use.
It should be noted that the above examples are only for further illustration and description of the technical solution of the present invention, and are not intended to further limit the technical solution of the present invention, and the method of the present invention is only a preferred embodiment, and is not intended to limit the protection scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The carbon black pore liquid is characterized by being a suspension liquid with the pH value of 9.8-10.6, which is prepared by mixing the following raw materials in percentage by weight:
wherein the film forming agent is selected from at least one of benzyl alcohol, dodecyl alcohol ester, ethylene glycol butyl ether, propylene glycol methyl ether, propylene glycol ethyl ether, propylene glycol butyl ether and propylene glycol phenyl ether, and the emulsifier is selected from anionic surfactant or nonionic surfactant;
the preparation method of the nano-scale carbon black comprises the following steps: adding concentrated sulfuric acid into carbon black prepared by a gas black method, stirring and soaking for 2-3h, then adding deionized water for dilution, removing acid liquor, adding ammonia water for neutralizing residual acid liquor until the pH value is greater than 7, carrying out centrifugal separation, then carrying out immersion washing and centrifugal separation treatment for multiple times by using deionized water, and when the pH value is detected to be 7-9, drying and dehydrating and grinding until the average particle size is not greater than 200nm to obtain carbon black powder; removing impurity iron from the carbon black powder to obtain the nano-scale carbon black.
2. The carbon black pore liquid according to claim 1, is a suspension with a pH of 9.8-10.6, which is prepared by mixing the following raw materials in percentage by weight:
3. the carbon black bore fluid according to claim 1 or 2, wherein the thickener is at least one selected from the group consisting of methylcellulose, hydroxyethylcellulose, hydroxypropylmethylcellulose, sodium carboxymethylcellulose, polyvinyl alcohol, sodium alginate polyacrylate, polyacrylamide, polyvinylpyrrolidone, polyethylene oxide, carbomer resin, and polyacrylic acid.
4. The carbon black bore fluid according to claim 1 or 2, wherein the pH adjusting agent is at least one selected from the group consisting of potassium carbonate, sodium bicarbonate, potassium bicarbonate, ammonia water, and ethanolamine.
5. The carbon black bore fluid according to claim 1 or 2, wherein the emulsifier is at least one selected from the group consisting of sulfate type anionic surfactants, sulfonate type anionic surfactants, and carboxylate type anionic surfactants.
6. The carbon black pore liquid according to claim 1 or 2, wherein the nonionic surfactant is at least one selected from fatty alcohol polyoxyethylene ether, alkylphenol ethoxylate, fatty acid polyoxyethylene ester, and castor oil polyoxyethylene ether.
7. The carbon black pore liquid according to claim 1 or 2, wherein the bactericide is at least one selected from the group consisting of s-triazines and isothiazolinone bactericides.
8. The method for producing the carbon black pore liquid according to any one of claims 1 to 7, characterized by comprising the steps of:
respectively preparing a film forming agent aqueous solution and a thickening agent aqueous solution, uniformly mixing the film forming agent aqueous solution and the thickening agent aqueous solution, and adding the rest water to form an intermediate mixed solution;
adding an emulsifier and an acid-base regulator into the intermediate mixed solution, uniformly stirring, adding nano-scale carbon black, shearing, stirring and dispersing to form a suspension;
grinding the suspension, and controlling the particle size range to be 140-180nm to obtain the material.
9. The method for preparing carbon black pore liquid according to claim 8, wherein the shearing and stirring process parameters are as follows: the rotating speed is not lower than 2000r/min, and the shearing dispersion time is not lower than 2 h.
10. A black hole process is characterized by comprising the following steps: providing a sample plate to be subjected to black hole treatment, and performing treatment by using the carbon black pore liquid according to any one of claims 1 to 7 by matching with the processes of micro etching, cleaning, water washing, pore finishing and plate drying.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115594171A (en) * | 2022-07-29 | 2023-01-13 | 广东利尔化学有限公司（Cn） | Carbon pore process nano graphite dispersion liquid and preparation method thereof |
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