CN113980753B - Leavening agent for high-speed plates and common plates and preparation method thereof - Google Patents

Leavening agent for high-speed plates and common plates and preparation method thereof Download PDF

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Publication number
CN113980753B
CN113980753B CN202111248406.8A CN202111248406A CN113980753B CN 113980753 B CN113980753 B CN 113980753B CN 202111248406 A CN202111248406 A CN 202111248406A CN 113980753 B CN113980753 B CN 113980753B
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leavening agent
novel
deionized water
plates
preparation
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CN113980753A (en
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蒋文明
宋胜
蔡志浩
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Jiangxi Chaoyang Technology Co ltd
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Jiangxi Chaoyang Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22Organic compounds
    • C11D7/36Organic compounds containing phosphorus
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22Organic compounds
    • C11D7/26Organic compounds containing oxygen
    • C11D7/261Alcohols; Phenols
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22Organic compounds
    • C11D7/26Organic compounds containing oxygen
    • C11D7/263Ethers
    • 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
    • C23C18/2053Pretreatment 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 only one step pretreatment
    • C23C18/2066Use of organic or inorganic compounds other than metals, e.g. activation, sensitisation with polymers
    • 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
    • C23C18/31Coating with metals
    • C23C18/38Coating with copper
    • 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
    • H05K3/0085Apparatus for treatments of printed circuits with liquids not provided for in groups H05K3/02 - H05K3/46; conveyors and holding means therefor
    • 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
    • H05K3/40Forming printed elements for providing electric connections to or between printed circuits
    • H05K3/42Plated through-holes or plated via connections
    • C11D2111/22

Abstract

The invention belongs to the technical field of chemical plating pretreatment, and particularly relates to a novel leavening agent and a preparation method thereof. The leavening agent comprises the following components in percentage by mass: alcohol ethers 40-50g/L; 15-20g/L of alcohols; 30-40g/L of alkali; 2-4g/L of inorganic polybasic acid; the balance of deionized water. The novel leavening agent disclosed by the invention takes alcohol ether as a solvent, can achieve the biting ability of the traditional leavening agent at a lower operation temperature in a short time under a low solvent condition, solves the problems that the biting amount of the novel material is insufficient, the pore wall separation is easy to cause, the tank liquor is clear under a high-concentration alkali condition and the novel leavening agent is mutually soluble with the alcohol ether leavening agent, and has the advantages of economic preparation and use cost, safety and environmental friendliness, can be used for treating various base materials, and has wide applicability.

Description

Leavening agent for high-speed plates and common plates and preparation method thereof
Technical Field
The invention belongs to the technical field of chemical plating pretreatment, and particularly relates to a leavening agent for high-speed plates and common plates and a preparation method thereof.
Background
With the progress of technology, new materials (such as high-speed plates) used in PCBs now have higher and higher requirements on drilling roughness, and especially hole wall binding force becomes a major problem. The holes are cracked between the resin and the glass fiber, and the cracks can remain the leavening agent, so that the spot-shaped or sheet-shaped hole wall floats off after the leavening agent naturally volatilizes. Therefore, it is desirable to minimize the solvent content in the vat, while minimizing the time required to minimize solvent residue.
The requirement for leavening agents is increasing, while shortening the leavening time and reducing the solvent while ensuring a certain amount of photoresist removal to prevent the formation of inter-level interconnect defects (ICDs). At present, in the process of removing the glue residues by using the traditional leavening agent, due to the appearance of a novel base material, the traditional leavening agent cannot remove molten glue residues and fragments by a glue residue removing process, so that the problems of weak biting force, easiness in residue, easiness in hole wall floating and the like of the clean hole wall resin surface and the reliable inner copper surface are provided. In addition, the traditional leavening agent has short service cycle, and the tank liquor is easy to be turbid and layered under the high-concentration alkali condition. This series of problems necessitates the development of a leavening agent that can be adapted to the new material.
Although Chinese patent CN113088410A provides an amide horizontal copper deposition leavening agent and a preparation method thereof, the patent uses amide substances, and the solvent is easy to volatilize, so that VOC emission is easy to cause; chinese patent CN106010830A provides a water-based swelling agent for a PCB and a use method thereof, but the method uses high solvent content as raw materials, so that the problem of poor adhesive force such as foaming or layering between a base material and a copper layer is easily caused in a fine seam between glass fiber and resin scraps by a solvent.
Disclosure of Invention
The invention aims to provide a novel leavening agent and a preparation method thereof, wherein the novel leavening agent can reach the biting ability of the traditional leavening agent at a lower operation temperature in a short time under the condition of low solvent, solves the problems that the biting amount of novel materials is insufficient and the pore wall separation is easy to cause, and the tank liquor is clear and the novel leavening agent is mutually soluble with alcohol ether leavening agent under the condition of high concentration alkali, and has the advantages of economic preparation and use cost, safe production and environmental friendliness.
The invention provides a novel leavening agent, which comprises the following components in percentage by mass:
alcohol ethers 40-50g/L;
15-20g/L of alcohols;
30-40g/L of alkali;
2-4g/L of inorganic polybasic acid;
the balance of deionized water.
According to the technical scheme, the solvent with low solvent content is used, so that the problem that the solvent causes poor adhesive force such as foaming or layering between a base material and copper layers in a fine seam between glass fiber and resin scraps can be solved, the vapor pressure of the alcohol ether type leavening agent is lower than that of amides, the problem of heat reliability and solvent volatilization are not easy to occur, and the problem of failure of the anode conductive wire is facilitated to be relieved.
Further, in the above technical scheme, the alcohol ether includes one or more of benzyl alcohol butyl ether, diethylene glycol monobutyl ether, triethylene glycol butyl ether and tripropylene glycol butyl ether. In the technical scheme, the ether is used as a solvent of the leavening agent, so that various base materials can be inflated and softened.
Further, in the above technical solution, the alcohol includes one or more of 1, 4-butanediol, glycerol, and butanol. In the technical scheme, alcohols are adopted as wetting agents and cosolvents.
Further, in the above technical scheme, the inorganic polybasic acid is any one of phosphoric acid and phosphorous acid. The polybasic acid is added in the technical scheme, so that the buffer effect of the pH of the bath solution can be achieved, and the bath solution is free from layering phenomenon after the alkali is continuously added.
Further, in the above technical scheme, the alkali is any one of sodium hydroxide, potassium hydroxide or lithium hydroxide. In the technical scheme, strong alkali is used to provide a required strong alkaline environment for removing the gumming slag, and the gumming slag removing effect is good.
The invention also provides a preparation method of the novel leavening agent, which comprises the following steps: adding alcohol ethers into a container, adding deionized water, stirring uniformly, adding alcohols, stirring uniformly, adding inorganic polybasic acid, stirring uniformly, cooling to normal temperature, adding strong base, stirring uniformly, and fixing volume with deionized water to obtain the novel leavening agent liquid.
The invention also provides a using method of the novel leavening agent, which comprises the following steps: preparing a novel leavening agent according to a proportion, heating to 60-80 ℃, and then placing the PCB double-sided board or the multi-sided board into the novel leavening agent for soaking reaction for 6-9 min.
The novel leavening agent obtained in the technical scheme can obtain the required biting amount by only heating to a lower temperature and processing for 1-2 times when in use, reduces the consumption of energy sources, and is applicable to various base materials and wide in applicability.
Further, in the above technical scheme, when the PCB double-sided board or multi-layer board is a high-speed board material, the heating temperature is 70-80 ℃.
Further, in the above technical scheme, when the PCB double-sided board or the multi-layer board is a common board material, the heating temperature is 60-70 ℃.
Furthermore, the required biting amount can be achieved by using the technical scheme for 1-2 times.
Compared with the prior art, the beneficial effects are that:
1. the novel leavening agent disclosed by the invention takes alcohol ethers as a solvent, has lower vapor pressure than amides, is not easy to cause the problem of heat reliability, is beneficial to relieving the problem of failure of anode conductive wires, can be used for treating various base materials, and has wide applicability;
2. the invention adopts the solution with low solvent content, can reduce the problem of poor adhesive force such as foaming or layering between the base material and copper layer caused by the solvent in the fine seam between the glass fiber and the resin scraps, can reach the biting ability of the traditional leavening agent in a short time, and simultaneously adopts the leavening agent with low solvent content, thereby reducing the emission of waste gas COD and having low waste water treatment cost;
3. the method uses polybasic acid as the pH buffer of the tank liquor, so that the problem of clarification of the tank liquor and mutual dissolution of the tank liquor and alcohol ether leavening agents under the condition of high concentration alkali is solved;
4. when the novel leavening agent is used, the required biting amount can be achieved by only needing lower operation temperature and processing for 1-2 times, so that the consumption of energy sources is reduced;
5. the novel leavening agent solves the problems of insufficient biting amount of the novel material and easy hole wall separation, and has the advantages of low cost, safe production and environmental friendliness.
Detailed Description
The experimental methods in the following examples are conventional methods unless otherwise specified. The raw materials used in the following examples are all commercially available and commercially available unless otherwise specified.
The above technical features of the present invention and the technical features specifically described in the following (embodiment) may be combined with each other to form a new or preferred technical solution.
In order to make the technical solutions and advantages of the present invention more apparent, the following examples of the present invention will be combined, and only the technical solutions of the present invention will be further apparent and complete, and it should be noted that the fact that the description is an embodiment of the present invention does not represent all the solutions, and states: based on the embodiment of the invention, the invention belongs to the protection scope of the invention.
Example 1
A preparation method of a novel leavening agent comprises the following specific steps:
45g of diethylene glycol monobutyl ether is added into a beaker, 500mL of deionized water is added, stirring is carried out until the diethylene glycol monobutyl ether is completely dissolved, then 16g of 1, 4-butanediol and 3g of phosphoric acid are added, after the diethylene glycol monobutyl ether is uniformly stirred and completely dissolved, 35g of caustic soda flakes are added, and after the diethylene glycol monobutyl ether is uniformly stirred, deionized water is used for fixing the volume to 1L, thus obtaining the novel leavening agent solution.
Example 2
A preparation method of a novel leavening agent comprises the following specific steps:
adding 40g of triethylene glycol butyl ether into a beaker, adding 500mL of deionized water, stirring until the triethylene glycol butyl ether is completely dissolved, then adding 15g of glycerol and 2g of phosphorous acid, after the triethylene glycol butyl ether is uniformly stirred and completely dissolved, adding 30g of caustic soda flakes, uniformly stirring, and then using the deionized water to fix the volume to 1L to prepare the novel leavening agent solution.
Example 3
A preparation method of a novel leavening agent comprises the following specific steps:
50g of diethylene glycol-butyl ether is added into a beaker, 500mL of deionized water is added, stirring is carried out until complete dissolution, then 20g of butanol and 4g of phosphoric acid are added, after stirring is carried out uniformly and complete dissolution is carried out, 40g of potassium hydroxide is added, stirring is carried out uniformly, and deionized water is used for fixing volume to 1L, thus obtaining the novel leavening agent solution.
Test example 1
The novel leavening agent solution prepared in example 1 was used for treating medium and high TG panels (EM 825, IT158, S1000, IT 180A) by the following method: the novel leavening agent solution of example 1 was heated to 75 ℃, placed into a high TG panel in PCB, and allowed to react for 6min by soaking. The specific parameters are as follows:
(1) Parameters of the leavening cylinder:
novel leavening agent: 120mL/L;
sodium hydroxide: 35g/L;
temperature: 75 ℃;
time: 6min;
clear, colorless, free of turbidity, and free of turbidity even when heated continuously for 3 hours.
(2) Parameters of the rubber removing cylinder:
temperature: 75 ℃;
time: 18min;
potassium permanganate: 60g/L;
sodium hydroxide: 45g/L;
hexavalent manganese: 26g/L.
Test results: as shown in table 1.
TABLE 1
From the test results of table 1, it can be seen that the novel panels with medium and high TG can meet the requirement of the biting amount only by once treatment with the novel leavening agent of the present invention.
Test example 2
The novel leavening agent solution prepared in the embodiment 1 is used for treating common plates, and the treatment method comprises the following steps: the novel leavening agent solution in the embodiment 1 is heated to 70 ℃, and three common PCB boards are put into the leavening agent solution to be soaked and reacted for 6min and 8min respectively. The specific parameters are as follows:
(1) Parameters of the leavening cylinder:
novel leavening agent: 120mL/L;
sodium hydroxide: 35g/L;
temperature: 70 ℃;
time: 6min/8min/10min;
clear, colorless, free of turbidity, and free of turbidity even when heated continuously for 3 hours.
(2) Parameters of the rubber removing cylinder:
temperature: 75 ℃;
time: 18min;
potassium permanganate: 60g/L;
sodium hydroxide: 45g/L;
hexavalent manganese: 26g/L.
Test results: as shown in table 2.
TABLE 2
From the test results in table 2, it can be seen that the novel leavening agent used for soaking the PCB board material can meet the requirements of glue removal, but has little influence on the glue removal when the processing is carried out for 6 minutes or more, so that the excellent effect can be achieved only by selecting and processing for 6 minutes, the consumption of energy sources can be reduced, and the cost is reduced.
Test example 3
The novel leavening agent solution prepared in the embodiment 1 is used for treating common plates, and the treatment method comprises the following steps: the novel leavening agent solutions of example 1 were heated to 65 ℃, 70 ℃, 75 ℃, 80 ℃ respectively, and placed into the common PCB slabs respectively, and soaked for 6min respectively. The specific parameters are as follows:
(1) Parameters of the leavening cylinder:
novel leavening agent: 120mL/L;
sodium hydroxide: 35g/L;
temperature: 65 ℃/70 ℃/75 ℃/80 ℃;
time: 6min;
clear, colorless, free of turbidity, and free of turbidity even when heated continuously for 3 hours.
(2) Parameters of the rubber removing cylinder:
temperature: 75 ℃;
time: 18min;
potassium permanganate: 60g/L;
sodium hydroxide: 45g/L;
hexavalent manganese: 26g/L.
Test results: as shown in table 3.
TABLE 3 Table 3
As can be seen from the test results of Table 3, the temperature difference will affect the removal of the glue when the novel leavening agent of the present invention is used to soak the common PCB board material, but the removal of the glue will also increase with the increasing temperature. Therefore, for processing a common sheet material of a PCB, a processing temperature of 65-70 ℃ is preferable.
In conclusion, the novel leavening agent can reach the biting and etching capability of the traditional leavening agent at a lower temperature in a short time under the condition of low solvent, so that the consumption of energy sources can be reduced, and meanwhile, the leavening agent with low solvent content is used, so that the emission of waste gas COD is reduced.
Finally, it should be emphasized that the foregoing description is merely illustrative of the preferred embodiments of the invention, and that various changes and modifications can be made by those skilled in the art without departing from the spirit and principles of the invention, and any such modifications, equivalents, improvements, etc. are intended to be included within the scope of the invention.

Claims (6)

1. The leavening agent for the high-speed plate and the common plate is characterized by comprising the following components in mass concentration:
alcohol ethers 40-50g/L;
15-20g/L of alcohols;
30-40g/L of alkali;
2-4g/L of inorganic polybasic acid;
the balance of deionized water;
the alcohol ether comprises one or more of benzyl alcohol butyl ether, diethylene glycol monobutyl ether, triethylene glycol butyl ether and tripropylene glycol butyl ether;
the alcohols comprise one or more of 1, 4-butanediol, glycerol and butanol;
the alkali is any one of sodium hydroxide, potassium hydroxide or lithium hydroxide;
the inorganic polybasic acid is any one of phosphoric acid and phosphorous acid.
2. The method for preparing the leavening agent for high-speed plates and common plates according to claim 1, wherein the method comprises the following steps: adding alcohol ethers into a container, adding deionized water, stirring uniformly, adding alcohols, stirring uniformly, adding inorganic polybasic acid, stirring uniformly, cooling to normal temperature, adding strong base, stirring uniformly, and fixing volume with deionized water to obtain the leavening agent liquid.
3. A method of using the leavening agent of claim 1 or prepared from the leavening agent of claim 2, wherein the method of using is: preparing a leavening agent according to a proportion, heating to 60-80 ℃, and then placing the PCB double-sided board or the multi-sided board into the leavening agent for soaking reaction for 6-9 min.
4. The method of claim 3, wherein the heating temperature is 70-80 ℃.
5. The method of claim 3, wherein the heating temperature is 60-70 ℃.
6. The method of using a leavening agent of any one of claims 3 to 5 wherein the desired level of bite is achieved by 1 to 2 applications.
CN202111248406.8A 2021-10-26 2021-10-26 Leavening agent for high-speed plates and common plates and preparation method thereof Active CN113980753B (en)

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CN114133994A (en) * 2021-11-19 2022-03-04 广东世运电路科技股份有限公司 Swelling agent for manufacturing printed circuit board

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Publication number Priority date Publication date Assignee Title
KR20050024969A (en) * 2003-09-05 2005-03-11 삼성전기주식회사 Composition for brown oxide pretreatment having cleaning strength and adhesive strength of polyimide, and process for improving the adhesive strength of polyimide through brown oxide process
TW200712105A (en) * 2005-09-30 2007-04-01 Taiwan Uyemura Co Ltd The leavening agent
CN106010830A (en) * 2016-07-05 2016-10-12 昆山艾森半导体材料有限公司 Water-based leavening agent for PCB and use method of water-based leavening agent
CN113293362A (en) * 2021-05-25 2021-08-24 吉安宏达秋科技有限公司 Chemical copper plating bulking solution and preparation method and application thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20050024969A (en) * 2003-09-05 2005-03-11 삼성전기주식회사 Composition for brown oxide pretreatment having cleaning strength and adhesive strength of polyimide, and process for improving the adhesive strength of polyimide through brown oxide process
TW200712105A (en) * 2005-09-30 2007-04-01 Taiwan Uyemura Co Ltd The leavening agent
CN106010830A (en) * 2016-07-05 2016-10-12 昆山艾森半导体材料有限公司 Water-based leavening agent for PCB and use method of water-based leavening agent
CN113293362A (en) * 2021-05-25 2021-08-24 吉安宏达秋科技有限公司 Chemical copper plating bulking solution and preparation method and application thereof

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