CN115029749A - Alkaline pore-finishing agent and application thereof - Google Patents
Alkaline pore-finishing agent and application thereof Download PDFInfo
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- CN115029749A CN115029749A CN202210612794.1A CN202210612794A CN115029749A CN 115029749 A CN115029749 A CN 115029749A CN 202210612794 A CN202210612794 A CN 202210612794A CN 115029749 A CN115029749 A CN 115029749A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
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- Chemical Kinetics & Catalysis (AREA)
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- Automation & Control Theory (AREA)
- Manufacturing Of Printed Wiring (AREA)
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Abstract
The invention provides an alkaline pore-adjusting agent, which comprises the following components: the pH regulator comprises a pH regulator, a cationic surfactant and an anionic surfactant, wherein the anionic surfactant is a phosphate compound. The alkaline pore-finishing agent used in the invention adopts special anion and cation combination to form an amphoteric surfactant, the cations are distributed in pores in a section through electrostatic adsorption, the anions are blocked, and the charges in the pores are anions. The surface active agent can improve the surface tension of the liquid, so that the charge distribution in the holes is more uniform and compact, and a good adhesion base is provided for the subsequent adsorption of positive charge ion palladium.
Description
Technical Field
The invention belongs to the technical field of printed boards, and particularly relates to an alkaline pore-finishing agent and application thereof.
Background
Pcb (printed circuit board), i.e. printed circuit board, printed circuit board for short, is one of important parts in the electronic industry, is a support for electronic components, and is a carrier for electrical interconnection of electronic components. Almost every kind of electronic equipment, as small as electronic watches, calculators, as large as computers, communication electronics, military weaponry systems, has electronic components such as integrated circuits, and printed boards are used to electrically interconnect the various components.
The important through hole metallization process comprises the following process flows:
pinx → water washing → skim latex → water washing → neutralization → water washing → whole hole → water washing → presoaking → ionic palladium activation → water washing → reduction → water washing → electroless copper plating solution → water washing → drying → oil removal → acid washing → acidic copper plating.
With the increasing social demands for environmental protection and occupational health, the process of hole metallization (copper deposition) has been shifted from the traditional open gas unstructured emission vertical copper deposition equipment to the closed, directional emission horizontal equipment. The colloidal palladium catalyst in the vertical process cannot be applied to a liquid medicine exchange mode of high-speed circulating water bed falling of horizontal equipment due to the defect that the colloidal palladium catalyst is easily oxidized and decomposed when contacting air, and a more stable ionic palladium catalyst is produced. The PCB plate is naturally provided with negative charges due to material characteristics after drilling, colloid palladium ions are negatively charged in the vertical copper deposition process to be not beneficial to adsorption of colloid palladium, the negative charges in the holes need to be adjusted to be positive charges through a cation surfactant special for a hole-shaping process, an ion palladium catalyst is positively charged in the horizontal copper deposition process, and the traditional cation pore-shaping agent is not suitable any more.
Disclosure of Invention
The invention aims to provide an alkaline pore-forming agent and application thereof in order to solve the defects of the technology.
The invention provides an alkaline pore-adjusting agent in a first aspect, which comprises the following components: a pH adjuster, a cationic surfactant, and an anionic surfactant.
As one of preferable embodiments, wherein the anionic surfactant is a phosphate ester compound.
In a preferred embodiment, the cationic surfactant is an organic cationic surfactant.
Preferably, the PH adjusting agent is selected from: one or more of a hydroxide, a carbonate, or an ammonium salt.
Preferably, the PH adjusting agent is selected from: sodium hydroxide or potassium hydroxide.
As one of the preferable schemes, the cationic surfactant is selected from one or more of guanidine hydrochloride and alcohol amine.
Preferably, the alcohol amine is selected from methanolamine, ethanolamine, diethanolamine, triethanolamine, triisopropanolamine or tributanolamine.
In a preferred embodiment, the phosphate ester compound is one or more selected from alkyl phosphate, fatty alcohol-polyoxyethylene ether phosphate or phenol-polyoxyethylene ether phosphate.
As one of the preferable schemes, the alkyl phosphate is selected from monoalkyl phosphate, dialkyl phosphate or trialkyl phosphate.
As one of preferable embodiments, the alkyl phosphate is dimethyl phosphate, diethyl phosphate, dipropyl phosphate, dibutyl phosphate, trimethyl phosphate, triethyl phosphate, tripropyl phosphate or tributyl phosphate.
As one preferable scheme, the fatty alcohol polyoxyethylene ether phosphate is selected from isooctanol polyoxyethylene ether phosphate, tridecanol polyoxyethylene ether phosphate and the like.
Preferably, the phenol polyoxyethylene ether phosphate is selected from nonylphenol polyoxyethylene ether phosphate, tristylethylphenol polyoxyethylene ether phosphate, and the like.
As one of the preferable schemes, the material composition is as follows according to the mass percentage: 0.1-5% of PH regulator, 0.01-0.5% of cationic surfactant and 0.01-0.5% of anionic surfactant.
As one of the preferred schemes, the material composition is as follows according to the mass percentage: 0.1-2% of pH regulator, 0.05-0.5% of cationic surfactant and 0.05-0.5% of anionic surfactant.
As one of the preferred schemes, the material composition is as follows according to the mass percentage: 0.1-1% of pH regulator, 0.1-0.5% of cationic surfactant and 0.1-0.5% of anionic surfactant.
Preferably, the pore-adjusting agent further comprises polyethylene polyamine.
Preferably, the polyethylene polyamine is selected from one or more of diethylenetriamine, triethylenetetramine and tetraethylenepentamine.
In a preferred embodiment, the polyethylene polyamine is present in an amount of 1 to 10% by mass.
As one of the preferable schemes, the mass percent of the polyethylene polyamine is 1-5%
In a second aspect, the invention provides the use of the alkaline pore-modifying agent provided by the first aspect, wherein the use comprises the preparation and treatment processes of PCB plates.
The main contributions of the present invention with respect to the prior art are the following:
(1) the alkaline pore-finishing agent used in the invention adopts special anion and cation combination to form an amphoteric surfactant, cations are distributed in pores in a section through electrostatic adsorption, anions are blocked, and charges in the pores are anions. The surface active agent can improve the surface tension of the liquid, so that the charge distribution in the holes is more uniform and compact, and a good attachment base is provided for the subsequent adsorption of positive charge ion palladium.
(2) The alkaline pore-adjusting agent used in the invention is characterized by special anion and cation combination; is suitable for the charge adjustment in the pores of the ionic palladium activator; meanwhile, the treated activating agent is uniform and compact in adsorption and strong in adhesive force. Therefore, the technical scheme of the invention achieves unexpected technical effects.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present disclosure more apparent, the technical solutions of the embodiments of the present disclosure are clearly and completely described. It is to be understood that the described embodiments are only a few embodiments of the present disclosure, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the disclosure without any inventive step, are within the scope of protection of the disclosure.
1. The invention provides an alkaline pore-adjusting agent in a first aspect, which comprises the following components: a pH adjuster, a cationic surfactant, and an anionic surfactant.
As one of preferable embodiments, wherein the anionic surfactant is a phosphate ester compound.
In a preferred embodiment, the cationic surfactant is an organic cationic surfactant.
Preferably, the PH adjusting agent is selected from: one or more of a hydroxide, carbonate or ammonium salt.
Preferably, the PH adjusting agent is selected from: sodium hydroxide or potassium hydroxide.
As one of preferable embodiments, the cationic surfactant is selected from one or more of guanidine hydrochloride and alcohol amine.
Preferably, the alcohol amine is selected from methanolamine, ethanolamine, diethanolamine, triethanolamine, triisopropanolamine or tributanolamine.
In a preferred embodiment, the phosphate ester compound is one or more selected from alkyl phosphate, fatty alcohol-polyoxyethylene ether phosphate or phenol-polyoxyethylene ether phosphate.
As one of the preferable schemes, the alkyl phosphate is selected from monoalkyl phosphate, dialkyl phosphate or trialkyl phosphate.
As one of the preferable schemes, the alkyl phosphate is dimethyl phosphate, diethyl phosphate, dipropyl phosphate, dibutyl phosphate, trimethyl phosphate, triethyl phosphate, tripropyl phosphate or tributyl phosphate.
As one preferable scheme, the fatty alcohol polyoxyethylene ether phosphate is selected from isooctanol polyoxyethylene ether phosphate, tridecanol polyoxyethylene ether phosphate and the like.
Preferably, the phenol polyoxyethylene ether phosphate is selected from nonylphenol polyoxyethylene ether phosphate, tristylethylphenol polyoxyethylene ether phosphate, and the like.
As one of the preferable schemes, the material composition is as follows according to the mass percentage: 0.1-5% of PH regulator, 0.01-0.5% of cationic surfactant and 0.01-0.5% of anionic surfactant.
As one of the preferred schemes, the material composition is as follows according to the mass percentage: 0.1-2% of pH regulator, 0.01-0.1% of cationic surfactant and 0.05-0.1% of anionic surfactant.
As one of the preferred schemes, the material composition is as follows according to the mass percentage: 0.1-1% of pH regulator, 0.01-0.05% of cationic surfactant and 0.01-0.05% of anionic surfactant.
Preferably, the pore-adjusting agent further comprises polyethylene polyamine.
Preferably, the polyethylene polyamine is selected from one or more of diethylenetriamine, triethylenetetramine and tetraethylenepentamine.
In a preferred embodiment, the polyethylene polyamine is present in an amount of 1 to 10% by mass.
As one of preferable schemes, the mass percent of the polyethylene polyamine is 1-5%
2. In a second aspect, the invention provides the use of the alkaline pore-modifying agent provided in the first aspect, wherein the use comprises the processes of preparing and treating PCB plates.
3. The horizontal electroless copper plating process of the present invention is as follows (basic operation is in a conventional manner in the art):
pinus sylvestris 70 ℃ 60s → water washing → desmutting 80 ℃ 180s → water washing → neutralization 30 ℃ 60s → water washing → whole hole 50 ℃ 60s → water washing → presoaking 30 ℃ 20s → ionic palladium activation 50 ℃ 60s → water washing → reduction 40 ℃ 60s → water washing → electroless copper plating solution 35 ℃ 300s → water washing → drying → degreasing → acid washing → acidic electrolytic copper plating
4. The chemical copper plating performance verification method comprises the following steps:
deposition rate: using a light plate with a fixed size and without a copper-clad base material, taking out the light plate from a hole-trimming procedure to a chemical copper plating process, etching a copper-clad layer by using a microetching solution, and calculating the thickness of the copper-clad layer by a chemical titration method;
backlight detection: the method comprises the following steps of using a copper-clad PCB substrate with holes, taking out the PCB substrate from a Pensong process to a chemical plating process, taking a sample with a fixed size by using a sampling machine, cutting through holes in the sample to be half of full holes, observing the through holes through a lower light source in a metallographic microscope, and detecting the incompletely covered areas as light-transmitting bright points. Level 9 backlighting requires substantially complete coverage of the viewing target area, allowing 3-5 individual point-like transparent dots to exist.
5. Detailed description of the preferred embodiments
Example 1
A preparation method for realizing the special alkaline pore-adjusting agent comprises the following steps:
| component name | Mass percent |
| Sodium hydroxide | 0.5% |
| Diethylenetriamine | 5% |
| Ethanolamine | 0.02% |
| Phosphoric acid triethyl ester | 0.01% |
| Isooctanol polyoxyethylene ether phosphate | 0.01% |
| Guanidine hydrochloride | 0.02% |
Preparing working solution according to the proportion of 5% v/v, soaking at 40-60 ℃, washing → presoaking → ionic palladium adsorption → washing → reduction → washing → electroless copper plating, and performing backlight detection; the copper plating is uniform and compact, and the backlight is 9 grades, which shows that the pore-forming agent can well play the effects of adjusting charges and cleaning pore walls.
Example 2
A preparation method for realizing the special alkaline pore-adjusting agent comprises the following steps:
| component name | Mass percent of |
| Sodium hydroxide | 0.5% |
| Diethylenetriamine | 5% |
| Diethanolamine (DEA) | 0.03% |
| Phosphoric acid diethyl ester | 0.01% |
| Isooctanol polyoxyethylene ether phosphate | 0.01% |
Preparing working solution according to the proportion of 5% v/v, soaking at 40-60 ℃, washing → presoaking → ionic palladium adsorption → washing → reduction → washing → electroless copper plating, and performing backlight detection; the copper plating is uniform and compact, and the backlight is 9 grades, which shows that the pore-forming agent can well play the effects of adjusting charges and cleaning pore walls.
Example 3
A preparation method for realizing the special alkaline pore-adjusting agent comprises the following steps:
| component name | Mass percent |
| Sodium hydroxide | 0.5% |
| Triethylene tetramine | 3% |
| Triethanolamine | 0.01% |
| Phosphoric acid trimethyl ester | 0.01% |
| Isooctanol polyoxyethylene ether phosphate | 0.01% |
| Guanidine hydrochloride | 0.01% |
Preparing working solution according to the proportion of 5% v/v, soaking at 40-60 ℃, washing → presoaking → ionic palladium adsorption → washing → reduction → washing → electroless copper plating, and performing backlight detection; the copper plating is uniform and compact, and the backlight is 9 grades, which shows that the pore-forming agent can well play the effects of adjusting charges and cleaning pore walls.
Example 4
A preparation method for realizing the special alkaline pore-forming agent comprises the following steps:
| component name | Mass percent |
| Potassium hydroxide | 0.5% |
| Triethylene tetramine | 5% |
| Triethanolamine | 0.02% |
| Phosphoric acid dimethyl ester | 0.01% |
| Isooctanol polyoxyethylene ether phosphate | 0.01% |
Preparing working solution according to the proportion of 5% v/v, soaking at 40-60 ℃, washing → presoaking → ionic palladium adsorption → washing → reduction → washing → electroless copper plating, and performing backlight detection; the copper plating is uniform and compact, and the backlight is 9 grades, which shows that the pore-forming agent can well play the effects of adjusting charges and cleaning pore walls.
Example 5
A preparation method for realizing the special alkaline pore-adjusting agent comprises the following steps:
| component name | Mass percent of |
| Potassium hydroxide | 0.5% |
| Triethylene tetramine | 5% |
| Triisopropanolamine derivatives | 0.02% |
| Phosphoric acid triethyl ester | 0.01% |
| Isooctanol polyoxyethylene ether phosphate | 0.01% |
Preparing a working solution according to the proportion of 5% v/v, soaking at 40-60 ℃, washing with water → presoaking → ionic palladium adsorption → washing with water → reduction → washing with water → electroless copper plating, and performing backlight detection; the copper plating is uniform and compact, and the backlight is 9 grades, which shows that the pore-forming agent can well play the effects of adjusting charges and cleaning pore walls.
Example 6
A preparation method for realizing the special alkaline pore-forming agent comprises the following steps:
| component name | Mass percent of |
| Potassium hydroxide | 0.5% |
| Triethylene tetramine | 5% |
| Triisopropanolamine | 0.02% |
| Isooctanol polyoxyethylene ether phosphate | 0.02% |
Preparing working solution according to the proportion of 5% v/v, soaking at 40-60 ℃, washing → presoaking → ionic palladium adsorption → washing → reduction → washing → electroless copper plating, and performing backlight detection; the copper plating is uniform and compact, and the backlight is 9 grades, which shows that the pore-forming agent can well play the effects of adjusting charges and cleaning pore walls.
Comparative example 1
A preparation method for realizing the special alkaline pore-forming agent comprises the following steps:
| component name | Mass percent |
| Potassium hydroxide | 0.5% |
| Triethylene tetramine | 5% |
| Triisopropanolamine | 0.02% |
| Sodium dodecyl sulfate | 0.02% |
Preparing working solution according to the proportion of 5% v/v, soaking at 40-60 ℃, washing → presoaking → ionic palladium adsorption → washing → reduction → washing → electroless copper plating, and performing backlight detection; the backlight level is only 6 levels. The pore-regulating agent using sodium dodecyl sulfate as an anionic surfactant is far inferior to the phosphate surfactant in charge regulation and wall pore cleaning.
Comparative example 2
A preparation method for realizing the special alkaline pore-adjusting agent comprises the following steps:
| component name | Mass percent |
| Potassium hydroxide | 0.5% |
| Triethylene tetramine | 5% |
| Triisopropanolamine | 0.02% |
| Isooctanol polyoxyethylene ether phosphate | 0.01% |
| Sodium dodecyl sulfate | 0.01% |
Preparing working solution according to the proportion of 5% v/v, soaking at 40-60 ℃, washing → presoaking → ionic palladium adsorption → washing → reduction → washing → electroless copper plating, and performing backlight detection; the copper plating is uniform and compact, and the backlight is 8 grades, which shows that the pore-forming agent is improved in the effects of adjusting the charge and cleaning the pore wall after the phosphate surfactant is added on the basis of the comparative example 1.
Finally, it should be noted that: it should be understood that the above examples are only for clearly illustrating the present invention and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications are intended to be within the scope of the present invention.
Claims (10)
1. An alkaline pore-modifying agent comprises the following components: the pH regulator comprises a pH regulator, a cationic surfactant and an anionic surfactant, wherein the anionic surfactant is a phosphate compound.
2. An alkaline pore-modifying agent according to claim 1, wherein the cationic surfactant is an organic cationic surfactant.
3. An alkaline pore-forming agent according to claim 1 or 2, wherein the PH adjusting agent is selected from the group consisting of: one or more of a hydroxide, carbonate or ammonium salt.
4. An alkaline pore-modifying agent according to any one of claims 1 to 3, wherein the cationic surfactant is selected from one or more of guanidine hydrochloride and alcohol amine.
5. An alkaline pore-modifying agent as claimed in any one of claims 1 to 4, wherein the phosphate ester compound is selected from one or more of alkyl phosphate, fatty alcohol polyoxyethylene ether phosphate or phenol polyoxyethylene ether phosphate.
6. An alkaline pore-modifying agent according to claim 5, wherein the alkyl phosphate is selected from the group consisting of monoalkyl phosphate, dialkyl phosphate and trialkyl phosphate.
7. An alkaline pore-modifying agent according to any one of claims 1 to 6, consisting of, in mass percent: 0.1-5% of PH regulator, 0.01-0.5% of cationic surfactant and 0.01-0.5% of anionic surfactant.
8. A basic pore-modifying agent according to any one of claims 1 to 7, further comprising a polyethylene polyamine.
9. An alkaline pore-modifying agent according to claim 8, wherein the polyethylene polyamine is selected from one or more of diethylenetriamine, triethylenetetramine and tetraethylenepentamine.
10. Use of an alkaline conditioning agent according to any of claims 1 to 9 in the preparation or treatment of a PCB.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210612794.1A CN115029749B (en) | 2022-06-01 | 2022-06-01 | Alkaline pore-forming agent and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210612794.1A CN115029749B (en) | 2022-06-01 | 2022-06-01 | Alkaline pore-forming agent and application thereof |
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| CN115029749B CN115029749B (en) | 2023-06-09 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001247973A (en) * | 2000-03-06 | 2001-09-14 | C Uyemura & Co Ltd | Cleaning and conditioning agent and electroless copper plating method for printed circuit board |
| CN102758193A (en) * | 2012-07-31 | 2012-10-31 | 湖南利尔电子材料有限公司 | Electroless copper plating pretreatment solution used for high-frequency circuit board |
| CN107587138A (en) * | 2017-10-11 | 2018-01-16 | 湖南可盟新材料科技有限公司 | A kind of cleaning and conditioning agent for printed circuit board PTH |
| CN109825375A (en) * | 2019-02-26 | 2019-05-31 | 湖南互连微电子材料有限公司 | A kind of cleaning conditioner and its application method |
| CN110467975A (en) * | 2019-09-12 | 2019-11-19 | 北京恒信仝唯科技发展有限公司 | Cleaning agent and preparation method thereof |
-
2022
- 2022-06-01 CN CN202210612794.1A patent/CN115029749B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001247973A (en) * | 2000-03-06 | 2001-09-14 | C Uyemura & Co Ltd | Cleaning and conditioning agent and electroless copper plating method for printed circuit board |
| CN102758193A (en) * | 2012-07-31 | 2012-10-31 | 湖南利尔电子材料有限公司 | Electroless copper plating pretreatment solution used for high-frequency circuit board |
| CN107587138A (en) * | 2017-10-11 | 2018-01-16 | 湖南可盟新材料科技有限公司 | A kind of cleaning and conditioning agent for printed circuit board PTH |
| CN109825375A (en) * | 2019-02-26 | 2019-05-31 | 湖南互连微电子材料有限公司 | A kind of cleaning conditioner and its application method |
| CN110467975A (en) * | 2019-09-12 | 2019-11-19 | 北京恒信仝唯科技发展有限公司 | Cleaning agent and preparation method thereof |
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