CN111867269A - Manufacturing process of oil-removing pore-finishing agent for conducting hole of high-frequency plate and oil-removing pore-finishing process of oil-removing pore-finishing agent - Google Patents

Manufacturing process of oil-removing pore-finishing agent for conducting hole of high-frequency plate and oil-removing pore-finishing process of oil-removing pore-finishing agent Download PDF

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Publication number
CN111867269A
CN111867269A CN202010486280.7A CN202010486280A CN111867269A CN 111867269 A CN111867269 A CN 111867269A CN 202010486280 A CN202010486280 A CN 202010486280A CN 111867269 A CN111867269 A CN 111867269A
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Prior art keywords
pore
oil
finishing agent
finishing
washing
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董先友
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Dongguan Standard Electronic Material Co ltd
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Dongguan Standard Electronic Material Co ltd
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Priority to CN202010486280.7A priority Critical patent/CN111867269A/en
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    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00Apparatus or processes for manufacturing printed circuits
    • H05K3/22Secondary treatment of printed circuits
    • H05K3/26Cleaning or polishing of the conductive pattern
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18Pretreatment of the material to be coated
    • C23C18/20Pretreatment of the material to be coated of organic surfaces, e.g. resins
    • C23C18/2006Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30
    • C23C18/2046Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30 by chemical pretreatment
    • C23C18/2073Multistep pretreatment
    • C23C18/2086Multistep pretreatment with use of organic or inorganic compounds other than metals, first
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2203/00Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
    • H05K2203/07Treatments involving liquids, e.g. plating, rinsing
    • H05K2203/0779Treatments involving liquids, e.g. plating, rinsing characterised by the specific liquids involved
    • H05K2203/0783Using solvent, e.g. for cleaning; Regulating solvent content of pastes or coatings for adjusting the viscosity

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Printing Elements For Providing Electric Connections Between Printed Circuits (AREA)

Abstract

The invention discloses a manufacturing process of an oil removing and pore finishing agent for a via hole of a high-frequency plate and an oil removing and pore finishing process thereof, which comprises the steps of preparing a three-mouth flask, cleaning and drying the three-mouth flask by using deionized water, adding 100% tetrahydrofuran (anhydrous), introducing nitrogen after deoxidation and drying, then adding 5-15 wt% of naphthalene, stirring and dissolving the naphthalene, then cutting 0.5-4.5 wt% of metal sodium into small pieces, slowly stirring, adding the small pieces, continuously stirring until complete reaction is achieved, and forming a dark green naphthalene sodium solution in the three-mouth flask, namely the required oil removing and pore finishing agent; then placing the oil removing pore-finishing agent into a dry stainless steel oil removing pore-finishing groove, and introducing nitrogen into the pore-finishing groove; and (3) placing the high-frequency plate into the whole-hole groove, lasting for 3-5 minutes, taking out the high-frequency plate, washing with water, sequentially performing presoaking, catalysis, washing with water, acceleration, washing with water, copper precipitation, washing with water and drying with hot air, and finally turning to a full-plate copper plating process.

Description

Manufacturing process of oil-removing pore-finishing agent for conducting hole of high-frequency plate and oil-removing pore-finishing process of oil-removing pore-finishing agent
Technical Field
The invention belongs to the technical field of printed circuit board processing, and particularly relates to a manufacturing process of an oil removing and hole finishing agent for a via hole of a high-frequency board and an oil removing and hole finishing process of the oil removing and hole finishing agent.
Background
The existing degreasing and hole-trimming of the via hole metallization of the high-frequency printed circuit board (Teflon substrate) adopts a plasma treatment mode, the treatment mode has strict requirements on equipment, low production efficiency and poor treatment effect, and is not suitable for industrial large-scale production, so that the degreasing and hole-trimming of the via hole metallization of the high-frequency printed circuit board (Teflon substrate) urgently needs a manufacturing process for chemically treating the degreasing and hole-trimming, which is suitable for industrial large-scale production, simple in equipment requirement, high in production efficiency and good in treatment effect, to replace a plasma treatment process.
Disclosure of Invention
The invention provides a manufacturing process of an oil removing and pore finishing agent for a via hole of a high-frequency plate for solving the technical problems.
The solution adopted by the invention for realizing the technical effect is as follows:
the process for preparing the oil-removing pore-finishing agent for the via hole of the high-frequency plate comprises the following steps:
the method comprises the following steps: preparing a three-neck flask, washing and drying the three-neck flask by using deionized water;
step two: adding 100% tetrahydrofuran (anhydrous) into the three-neck flask;
step three: introducing nitrogen after deoxidation and drying into the three-neck flask;
step four: adding 5-15 wt% of naphthalene into the three-neck flask, and stirring and dissolving the naphthalene in the solution obtained in the third step;
Step five: cutting 0.5-4.5 wt% of metal sodium into small pieces, slowly stirring, adding into the three-neck flask, and continuously stirring the metal sodium to enable the metal sodium to completely react with the solution obtained in the fourth step, so as to form a dark green naphthalene sodium solution in the three-neck flask, namely the required oil removal pore-finishing agent.
Preferably, the deoxidation and drying process of the nitrogen in the step three is as follows: firstly introducing the nitrogen into a sealed buffer bottle, then sequentially introducing the nitrogen into a solution of 5-15 wt% of pyrogallic acid and 2-3 wt% of sodium hydroxide sealed in the buffer bottle for deoxidation, then passing through the sealed buffer bottle, and finally dehydrating in a sealed bottle filled with solid calcium oxide.
Preferably, in the fifth step, the temperature of the chemical reaction is 10 ℃ +/-5 ℃.
Preferably, the pH value of the oil removal pore-finishing agent is more than or equal to 12, and the specific gravity of the oil removal pore-finishing agent is 1.02-1.08g/cm3
The oil removing and hole finishing process of the conducting hole of the high-frequency plate comprises the following steps of:
the method comprises the following steps: placing the oil removing pore-finishing agent into a dry stainless steel oil removing pore-finishing groove, and introducing nitrogen into the pore-finishing groove;
step two: placing a high-frequency plate into the whole-hole groove for 3-5 minutes;
step three: taking out the high-frequency plate and washing with water;
Step four: sequentially carrying out presoaking, catalysis, washing, acceleration, washing, copper deposition, washing and hot air blow-drying treatment on the high-frequency plate, and then transferring to a whole plate copper plating process.
The invention has the beneficial effects that: (1) high-cost equipment investment is not needed; (2) the manufacturing process is simple and feasible; (3) the oil removal and hole trimming of the via hole of the high-frequency plate can be finished without expensive plasma equipment; (4) the production efficiency of oil removal and hole finishing of the via hole of the high-frequency plate is greatly improved (by more than ten times relatively); (5) the automatic production is convenient; (6) the backlight level of hole metallization of the via hole of the high-frequency board is improved, and the copper-free ratio of the via hole is reduced (which can reach 0.01% and is 5% after plasma treatment); (7) the quality reliability of the high-frequency board is improved (the phenomena of no hole/copper separation for 6 times at 288 ℃ after hole metallization copper plating, and the phenomena of no hole/copper separation for 3 times at 288 ℃ after the hole metallization copper plating after plasma treatment at 10S); (8) the raw materials have wide sources, low price, low cost and no pollution in the production process, so the method has wide application prospect in the field of printed circuit boards.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. It will be understood that when an element is referred to as being "secured to" or "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. When one element is referred to as being "fixedly attached" to another element, it can be fixedly attached by welding, bolting, gluing, or the like.
The invention discloses a process for preparing an oil removing and pore finishing agent for a via hole of a high-frequency plate in a preferred embodiment, which comprises the following steps:
the method comprises the following steps: preparing a three-neck flask, washing and drying the three-neck flask by using deionized water;
step two: adding 100% tetrahydrofuran (anhydrous) into the three-neck flask;
step three: introducing nitrogen after deoxidation and drying into the three-neck flask;
step four: adding 5-15 wt% of naphthalene into the three-neck flask, and stirring and dissolving the naphthalene in the solution obtained in the third step;
step five: cutting 0.5-4.5 wt% of metal sodium into small pieces, slowly stirring, adding into the three-neck flask, and continuously stirring the metal sodium to enable the metal sodium to completely react with the solution obtained in the fourth step, so as to form a dark green naphthalene sodium solution in the three-neck flask, namely the required oil removal pore-finishing agent.
Specifically, the deoxidation and drying process of the nitrogen in the third step is as follows: firstly introducing the nitrogen into a sealed buffer bottle, then sequentially introducing the nitrogen into a solution of 5-15 wt% of pyrogallic acid and 2-3 wt% of sodium hydroxide sealed in the buffer bottle for deoxidation, then passing through the sealed buffer bottle, and finally dehydrating in a sealed bottle filled with solid calcium oxide.
Specifically, in the fifth step, the temperature of the chemical reaction is 10 ℃ +/-5 ℃.
Specifically, the pH value of the oil removing pore-finishing agent is more than or equal to 12, and the specific gravity of the oil removing pore-finishing agent is 1.02-1.08g/cm3
The invention discloses an oil removing and hole finishing process of a via hole of a high-frequency plate in a preferred embodiment, which comprises the following steps:
the method comprises the following steps: placing the oil removing pore-finishing agent into a dry stainless steel oil removing pore-finishing groove, and introducing nitrogen into the pore-finishing groove;
step two: placing a high-frequency plate into the whole-hole groove for 3-5 minutes;
step three: taking out the high-frequency plate and washing with water;
step four: sequentially carrying out presoaking, catalysis, washing, acceleration, washing, copper deposition, washing and hot air blow-drying treatment on the high-frequency plate, and then transferring to a whole plate copper plating process.
Further, the high-frequency board detection results of the oil removal pore-finishing agent prepared by the process of the invention after completing metallization and electro-coppering after oil removal pore-finishing are as follows:
the first embodiment is as follows:
tetrahydrofuran: 100%, naphthalene: 10%, metallic sodium: 0.8 percent
The high-frequency plate finishes hole metallization and electrolytic copper plating after oil removal and hole trimming
Figure BDA0002519193640000031
Figure BDA0002519193640000041
Watch 1
Example two:
tetrahydrofuran: 100%, naphthalene: 15%, metallic sodium: 12 percent of
The high-frequency plate finishes hole metallization and electrolytic copper plating after oil removal and hole trimming
Figure BDA0002519193640000042
Watch two
According to experimental results, the hydrophilicity of a through hole of a high-frequency board can be improved by the high-frequency printed circuit board (a teflon substrate) treated by a chemical method, so that a catalyst layer is better and firmly attached to the hole wall, a copper layer on the hole wall after copper deposition can be more completely covered (backlight can reach more than 9 levels), the hole copper-free proportion of the high-frequency board is reduced, the copper deposition backlight treated by plasma can only reach 8 levels, the hole copper-free proportion is usually 0.5%, and the hole copper-free proportion treated by the oil-removing pore-finishing agent is reduced to 0.01%. Meanwhile, the bonding force between the copper-deposited layer and the hole wall of the via hole is improved, so that the quality defect of hole-copper separation is reduced to 0.05% from 3%.
While the preferred embodiments of the present invention have been illustrated and described in detail, it should be understood that the scope of the invention includes, but is not limited to, the embodiments described above; the particular arrangements disclosed in the specification are illustrative of preferred embodiments of the invention and other embodiments may be devised by those skilled in the art based on the teachings herein, and any such variations and equivalents may be resorted to without departing from the novel concepts of the invention.

Claims (5)

1. The manufacturing process of the oil removing and pore finishing agent for the via hole of the high-frequency plate is characterized by comprising the following steps of:
the method comprises the following steps: preparing a three-neck flask, washing and drying the three-neck flask by using deionized water;
step two: adding 100% tetrahydrofuran (anhydrous) into the three-neck flask;
step three: introducing nitrogen after deoxidation and drying into the three-neck flask;
step four: adding 5-15 wt% of naphthalene into the three-neck flask, and stirring and dissolving the naphthalene in the solution obtained in the third step;
step five: cutting 0.5-4.5 wt% of metal sodium into small pieces, slowly stirring, adding into the three-neck flask, and continuously stirring the metal sodium to enable the metal sodium to completely react with the solution obtained in the fourth step, so as to form a dark green naphthalene sodium solution in the three-neck flask, namely the required oil removal pore-finishing agent.
2. The process for producing an oil-removing pore-finishing agent for via holes of high-frequency plates as claimed in claim 1, wherein: the deoxidation and drying process of the nitrogen in the third step is as follows: firstly introducing the nitrogen into a sealed buffer bottle, then sequentially introducing the nitrogen into a solution of 5-15 wt% of pyrogallic acid and 2-3 wt% of sodium hydroxide sealed in the buffer bottle for deoxidation, then passing through the sealed buffer bottle, and finally dehydrating in a sealed bottle filled with solid calcium oxide.
3. The process for producing an oil-removing pore-finishing agent for via holes of high-frequency plates as claimed in claim 1, wherein: in the fifth step, the temperature of the chemical reaction is 10 +/-5 ℃.
4. The process for producing an oil-removing pore-finishing agent for via holes of high-frequency plates as claimed in claim 1, wherein: the pH value of the oil removing pore-finishing agent is more than or equal to 12, and the specific gravity of the oil removing pore-finishing agent is 1.02-1.08g/cm3
5. The oil removing and hole finishing process of the via hole of the high-frequency plate is characterized by comprising the following steps of:
the method comprises the following steps: placing the oil removing pore-finishing agent into a dry stainless steel oil removing pore-finishing groove, and introducing nitrogen into the pore-finishing groove;
step two: placing a high-frequency plate into the whole-hole groove for 3-5 minutes;
step three: taking out the high-frequency plate and washing with water;
step four: sequentially carrying out presoaking, catalysis, washing, acceleration, washing, copper deposition, washing and hot air blow-drying treatment on the high-frequency plate, and then transferring to a whole plate copper plating process.
CN202010486280.7A 2020-06-01 2020-06-01 Manufacturing process of oil-removing pore-finishing agent for conducting hole of high-frequency plate and oil-removing pore-finishing process of oil-removing pore-finishing agent Pending CN111867269A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101935404A (en) * 2009-06-30 2011-01-05 陈仕明 Naphthalizing treatment belt
TW201447036A (en) * 2013-03-14 2014-12-16 羅門哈斯電子材料有限公司 Method of filling through-holes
CN106827719A (en) * 2017-01-09 2017-06-13 三峡大学 A kind of high-frequency high-speed flexibility coat copper plate and preparation method thereof
CN109413858A (en) * 2018-11-09 2019-03-01 博罗康佳精密科技有限公司 A kind of preparation method of microwave ceramics substrate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101935404A (en) * 2009-06-30 2011-01-05 陈仕明 Naphthalizing treatment belt
TW201447036A (en) * 2013-03-14 2014-12-16 羅門哈斯電子材料有限公司 Method of filling through-holes
CN106827719A (en) * 2017-01-09 2017-06-13 三峡大学 A kind of high-frequency high-speed flexibility coat copper plate and preparation method thereof
CN109413858A (en) * 2018-11-09 2019-03-01 博罗康佳精密科技有限公司 A kind of preparation method of microwave ceramics substrate

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Application publication date: 20201030

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