CN114133994A - Swelling agent for manufacturing printed circuit board - Google Patents
Swelling agent for manufacturing printed circuit board Download PDFInfo
- Publication number
- CN114133994A CN114133994A CN202111375428.0A CN202111375428A CN114133994A CN 114133994 A CN114133994 A CN 114133994A CN 202111375428 A CN202111375428 A CN 202111375428A CN 114133994 A CN114133994 A CN 114133994A
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- Prior art keywords
- leavening agent
- monobutyl ether
- circuit board
- glycol monobutyl
- phosphoric acid
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- 230000008961 swelling Effects 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 235000010855 food raising agent Nutrition 0.000 claims abstract description 88
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 25
- 238000005553 drilling Methods 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical class CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims abstract description 12
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 claims description 25
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 24
- 238000007654 immersion Methods 0.000 claims description 6
- CUVLMZNMSPJDON-UHFFFAOYSA-N 1-(1-butoxypropan-2-yloxy)propan-2-ol Chemical compound CCCCOCC(C)OCC(C)O CUVLMZNMSPJDON-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- COBPKKZHLDDMTB-UHFFFAOYSA-N 2-[2-(2-butoxyethoxy)ethoxy]ethanol Chemical compound CCCCOCCOCCOCCO COBPKKZHLDDMTB-UHFFFAOYSA-N 0.000 claims description 2
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 2
- 230000009477 glass transition Effects 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract description 10
- 238000002360 preparation method Methods 0.000 abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 3
- 230000000996 additive effect Effects 0.000 abstract description 3
- 230000035699 permeability Effects 0.000 abstract description 3
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 30
- 238000012360 testing method Methods 0.000 description 16
- 239000003292 glue Substances 0.000 description 12
- 238000005406 washing Methods 0.000 description 10
- 239000000758 substrate Substances 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 230000008569 process Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000001465 metallisation Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 239000004642 Polyimide Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 229920001721 polyimide Polymers 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 150000002170 ethers Chemical class 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 230000002522 swelling effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/263—Ethers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/02—Inorganic compounds
- C11D7/04—Water-soluble compounds
- C11D7/08—Acids
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/261—Alcohols; Phenols
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/22—Electronic devices, e.g. PCBs or semiconductors
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Detergent Compositions (AREA)
- Manufacturing Of Printed Wiring (AREA)
Abstract
The invention discloses a swelling agent used in the manufacture of a printed circuit board. The leavening agent comprises the following components: monobutyl ether derivative, butanediol, phosphoric acid and water. The leavening agent is a formula of alcohol ether combination and phosphoric acid additive, and has lower volatility and excellent permeability; the preparation method is simple, green and safe, and the preparation can be completed at room temperature; the swelling agent can be widely applied to removing the drilling dirt of the circuit board.
Description
Technical Field
The invention belongs to the field of chemistry, and particularly relates to a swelling agent for manufacturing a printed circuit board.
Background
In the process of manufacturing printed circuit boards, in order to save space and weight, the circuit boards are often manufactured as two-layer or multi-layer printed circuit boards in cooperation with various electrical devices. Each circuit layer is separated from the other circuit layers by an insulating material, which is typically a resin-containing material such as epoxy, epoxy/fiberglass material, or polyimide. To conduct the circuit layers of different layers, drilling is required, and then the holes are metallized to form conductive paths. Because the resin in the printed board is melted by the high temperature during drilling, the resin adhesive is generated and is adhered to the surface of the conductor on the wall of the hole to form the drilling dirt. In this case, to maintain good electrical conductivity between the hole wall metallization and the metal conductor, the smear on the hole wall must be removed.
The existing method for removing the drilling stains by using the alkaline permanganate is divided into three working procedures: swelling, permanganate desmearing, neutralizing. Swelling is to soak the plate to be desmeared in swelling agent to make the desmear swell and partially dissolve, which creates favorable condition for the next desmear. Most of the existing leavening agents are single-component ether formulas, and the ethers are volatile at the operation temperature of 70 ℃, so that the environment is polluted and great harm is caused to operators. Therefore, it is necessary to develop a swelling agent having a good swelling effect and low volatility.
Disclosure of Invention
In order to overcome the problems of the prior art as described above, it is an object of the present invention to provide a leavening agent; the other purpose of the invention is to provide a preparation method of the leavening agent; it is a further object of the present invention to provide such leavening agent applications; the fourth objective of the present invention is to provide a method for removing circuit board drilling dirt.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
in a first aspect, the present invention provides a leavening agent comprising the following components: monobutyl ether derivative, butanediol, phosphoric acid and water.
Preferably, the monobutyl ether derivative comprises at least one of diethylene glycol monobutyl ether, triethylene glycol monobutyl ether, ethylene glycol monobutyl ether and dipropylene glycol monobutyl ether; further preferably, the monobutyl ether derivative comprises at least one of diethylene glycol monobutyl ether and dipropylene glycol monobutyl ether; still more preferably, the monobutyl ether derivative is diethylene glycol monobutyl ether.
Preferably, the butanediol is 1, 4-butanediol.
Preferably, the mass concentration of each component of the leavening agent is as follows:
5 g/L-120 g/L of monobutyl ether derivative;
5 g/L-30 g/L of butanediol;
1 g/L-6 g/L phosphoric acid;
further preferably, the mass concentration of each component of the leavening agent is as follows:
monobutyl ether derivative 20-80 g/L;
12 g/L-20 g/L of butanediol;
2 g/L-5 g/L phosphoric acid;
still further preferably, the mass concentration of each component of the leavening agent is as follows:
monobutyl ether derivative 40-60 g/L;
12 g/L-20 g/L of butanediol;
2 g/L-4 g/L phosphoric acid;
more preferably, the mass concentration of each component of the leavening agent is as follows:
monobutyl ether derivative 40-50 g/L;
12 g/L-20 g/L of butanediol;
2 g/L-4 g/L phosphoric acid.
Preferably, the glue removing rate of the leavening agent is 0.15mg/cm2-0.45mg/cm2(ii) a Further preferably, the glue removing rate of the leavening agent is 0.18mg/cm2-0.39mg/cm2(ii) a Still further preferably, the gel removal rate of the leavening agent is 0.22mg/cm2-0.39mg/cm2。
In a second aspect, the present invention provides a method for preparing the leavening agent according to the first aspect of the present invention, comprising the steps of:
and mixing the components to obtain the leavening agent.
In a third aspect, the present invention provides the use of the leavening agent according to the first aspect of the present invention for removing circuit board smear.
Preferably, the flame-retardant material grade of the circuit board is FR-4.
Preferably, the glass transition temperature (TG value) of the circuit board is 140-180 ℃.
Preferably, the circuit board is 8cm × 8cm in shape; further preferably, the circuit board has a shape of 6cm × 6 cm.
Preferably, the diameter of the drilled hole of the drilling dirt is 0.08mm-1.2 mm; further preferably, the diameter of the drilled hole of the drilling dirt is 0.1mm-1.0 mm; still further preferably, the bore diameter of the smear is 0.1mm to 0.9 mm.
Preferably, the depth of the drill hole with the drilling dirt is 1.2mm-2.0 mm; further preferably, the depth of the drill hole is 1.44mm to 1.76 mm.
Preferably, the circuit board is a circuit board comprising an epoxy resin or a polyimide.
The fourth aspect of the present invention provides a method for removing circuit board smear, comprising the steps of:
the circuit board is cleaned by immersing in a leavening agent according to the first aspect of the invention.
Preferably, the immersion temperature is 50-80 ℃; further preferably, the temperature of the immersion is 70 ℃ to 75 ℃.
Preferably, the immersion time is 4min-12 min; further preferably, the immersion time is 6min to 9 min.
Preferably, after the circuit board is immersed in the leavening agent, the method further comprises the step of removing glue from the circuit board by using alkaline permanganate.
The invention has the beneficial effects that:
the leavening agent is a formula of alcohol ether combination and phosphoric acid additive, and has lower volatility and excellent permeability; the preparation method is simple, green and safe, and the preparation can be completed at room temperature; the swelling agent can be widely applied to removing the drilling dirt of the circuit board.
Specifically, the invention has the following advantages:
1. the swelling agent provided by the invention is a formula of alcohol ether combination and phosphoric acid additive, can reduce the volatilization of ethers at the operation temperature of 70 ℃, and reduces the harm and environmental pollution to operators; compared with the traditional single-component ether leavening agent, the agent has stronger permeability, can effectively swell the residue left in the tiny hole wall in the multilayer printed circuit board with the TG value of 140-180 ℃, can better swell and partially dissolve the drilling dirt, and provides good conditions for subsequent removal of the drilling dirt and chemical copper deposition.
2. The leavening agent provided by the invention is simple in preparation method, green and safe, can be prepared at room temperature, and has the advantage of mass production.
3. The leavening agent provided by the invention is a pre-treatment leavening agent for removing the drilling dirt of alkaline permanganate in the manufacturing of printed circuit boards, has excellent swelling effect on the circuit boards containing epoxy resin and polyimide materials, and can be widely applied to the manufacturing of the circuit boards.
Drawings
FIG. 1 is a circuit board backlight level diagram.
Detailed Description
The following description of the embodiments of the present invention is provided in connection with the accompanying drawings and examples, but the invention is not limited thereto. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available through commercial purchase.
Example 1
The components of the leavening agent of this example are shown in Table 1.
Table 1: leavening agent component of example 1
The leavening agent of this example was prepared as follows: adding a proper amount of deionized water into a beaker, then sequentially adding 45g of diethylene glycol monobutyl ether, 16g of 1, 4-butanediol and 3g of phosphoric acid, uniformly stirring, and finally adding the balance of water to 1 liter to obtain the leavening agent prepared by the embodiment, wherein the leavening agent can enter a treatment use stage.
Example 2
The components of the leavening agent of this example are shown in Table 2.
Table 2: leavening agent component of example 2
Name of raw materials | Concentration of |
Diethylene glycol monobutyl ether | 20g/L |
1, 4-butanediol | 16g/L |
Phosphoric acid | 3g/L |
Pure water | Balance of |
The leavening agent of this example was prepared as follows: adding a proper amount of deionized water into a beaker, then sequentially adding 20g of diethylene glycol monobutyl ether, 16g of 1, 4-butanediol and 3g of phosphoric acid, uniformly stirring, and finally adding the balance of water to 1 liter to obtain the leavening agent prepared by the method, wherein the leavening agent can enter a treatment use stage.
Example 3
The components of the leavening agent of this example are shown in Table 3.
Table 3: leavening agent component of example 3
Name of raw materials | Concentration of |
Diethylene glycol monobutyl ether | 30g/L |
1, 4-butanediol | 16g/L |
Phosphoric acid | 3g/L |
Pure water | Balance of |
The leavening agent of this example was prepared as follows: adding a proper amount of deionized water into a beaker, then sequentially adding 30g of diethylene glycol monobutyl ether, 16g of 1, 4-butanediol and 3g of phosphoric acid, uniformly stirring, and finally adding the balance of water to 1 liter to obtain the leavening agent prepared by the embodiment, wherein the leavening agent can enter a treatment use stage.
Example 4
The components of the leavening agent of this example are shown in Table 4.
Table 4: leavening agent component of example 4
The leavening agent of this example was prepared as follows: adding a proper amount of deionized water into a beaker, then sequentially adding 40g of diethylene glycol monobutyl ether, 16g of 1, 4-butanediol and 3g of phosphoric acid, uniformly stirring, and finally adding the balance of water to 1 liter to obtain the leavening agent prepared by the method, wherein the leavening agent can enter a treatment use stage.
Example 5
The components of the leavening agent of this example are shown in Table 5.
Table 5: leavening agent component of example 5
Name of raw materials | Concentration of |
Diethylene glycol monobutyl ether | 50g/L |
1, 4-butanediol | 16g/L |
Phosphoric acid | 3g/L |
Pure water | Balance of |
The leavening agent of this example was prepared as follows: adding a proper amount of deionized water into a beaker, then sequentially adding 50g of diethylene glycol monobutyl ether, 16g of 1, 4-butanediol and 3g of phosphoric acid, uniformly stirring, and finally adding the balance of water to 1 liter to obtain the leavening agent prepared by the embodiment, wherein the leavening agent can enter a treatment use stage.
Example 6
The components of the leavening agent of this example are shown in Table 6.
Table 6: leavening agent component of example 3
Name of raw materials | Concentration of |
Diethylene glycol monobutyl ether | 60g/L |
1, 4-butanediol | 16g/L |
Phosphoric acid | 3g/L |
Pure water | Balance of |
The leavening agent of this example was prepared as follows: adding a proper amount of deionized water into a beaker, then sequentially adding 60g of diethylene glycol monobutyl ether, 16g of 1, 4-butanediol and 3g of phosphoric acid, uniformly stirring, and finally adding the balance of water to 1 liter to obtain the leavening agent prepared by the method, wherein the leavening agent can enter a treatment use stage.
Example 7
The components of the leavening agent of this example are shown in Table 7.
Table 7: leavening agent component of example 7
Name of raw materials | Concentration of |
Diethylene glycol monobutyl ether | 70g/L |
1, 4-butanediol | 16g/L |
Phosphoric acid | 3g/L |
Pure water | Balance of |
The leavening agent of this example was prepared as follows: adding a proper amount of deionized water into a beaker, then sequentially adding 70g of diethylene glycol monobutyl ether, 16g of 1, 4-butanediol and 3g of phosphoric acid, uniformly stirring, and finally adding the balance of water to 1 liter to obtain the leavening agent prepared by the method, wherein the leavening agent can enter a treatment use stage.
Example 8
The components of the leavening agent of this example are shown in Table 8.
Table 8: leavening agent component of example 8
Name of raw materials | Concentration of |
Diethylene glycol monobutyl ether | 80g/L |
1, 4-butanediol | 16g/L |
Phosphoric acid | 3g/L |
Pure water | Balance of |
The leavening agent of this example was prepared as follows: adding a proper amount of deionized water into a beaker, then sequentially adding 80g of diethylene glycol monobutyl ether, 16g of 1, 4-butanediol and 3g of phosphoric acid, uniformly stirring, and finally adding the balance of water to 1 liter to obtain the leavening agent prepared by the method, wherein the leavening agent can enter a treatment use stage.
Performance testing
The process flow of the invention is the same as the process flow of the chemical copper plating hole metallization of the traditional multilayer board and double-sided board, and the specific process flow is as follows: the method comprises the steps of (1) drilling and dirt swelling → water washing → alkaline permanganate degumming → water washing → acid neutralization → water washing → oil removal adjustment → water washing → micro-etching → water washing → pre-dipping treatment → activation treatment → water washing → acceleration treatment → water washing → electroless copper plating → water washing → drying.
The conditions for treating the multi-layer board and the double-sided board with the leavening agent are as follows: the circuit board is soaked in swelling agent in a swinging mode, the treatment temperature is 70-75 ℃, and the soaking time is 6-9 minutes.
1. Testing of glue removal rate of swelling agent on plates with different TG values
Taking a cut FR-4 substrate (flame-retardant material grade) with 6cm multiplied by 6cm and TG values of 140 ℃, 160 ℃ and 180 ℃ respectively, polishing the periphery with sand paper, cleaning, and baking in an oven at 120 +/-5 ℃ for 15 min; the mixture was taken out and cooled to room temperature in a desiccator, and weighed and recorded as W1 (accurate to 0.1 mg). Then using the leavening agent prepared in example 1, taking out the plate after going through the desmear process (from swelling to acid neutralization and then washing); cleaning, and baking in an oven at 120 + -5 deg.C for 15 min; the mixture was taken out and cooled to room temperature in a desiccator, and weighed and recorded as W2 (accurate to 0.1 mg).
Calculating the formula: glue removal rate (mg/cm)2) (W1-W2)/(2s) wherein: s is the substrate area (length x width) generally requiring a glue removal rate: 0.15mg/cm2-0.45mg/cm2. The test results are shown in table 9.
Table 9: example 1 results of gel removal rates of leavening agents for different TG value boards
Sheet material with different TG values | Treatment temperature (. degree.C.) | Soaking time (minutes) | Glue removal rate (mg/cm)2) |
TG value of 140 deg.C | 73 | 8 | 0.39 |
TG value of 160 ℃ C | 73 | 8 | 0.31 |
TG value of 180 deg.C | 73 | 8 | 0.22 |
Table 9 shows that the swelling agent prepared in example 1 of the present invention has a gel removal rate of 0.39mg/cm against a substrate having a TG value of 140 deg.C2The glue removing rate of the substrate with the TG value of 160 ℃ is 0.31mg/cm2The glue removing rate of the substrate with the TG value of 180 ℃ is 0.22mg/cm2. The test results show that the leavening agent prepared in example 1 of the present invention has excellent degumming rate for the substrate.
2. Gel removal Rate testing of leavening agents with varying concentrations of diethylene glycol monobutyl ether
The main component of the leavening agent provided by the invention is diethylene glycol monobutyl ether, and the part tests the degumming rate of the leavening agent under different concentrations of the diethylene glycol monobutyl ether. The test procedure was as follows:
the cut FR-4 substrate (6cm multiplied by 6cm) with the TG value of 160 ℃ is taken out, the leavening agents of the examples 2 to 8 are adopted, the substrate is taken out after going through the normal degumming procedure (from swelling to acid neutralization and then washing), the degumming rate of the substrate is calculated (the calculation method is shown as the performance test 1), and the test results are shown in the table 10.
Table 10: results of testing gel removal rate of different concentrations of diethylene glycol monobutyl ether for leavening agent
Table 10 shows that the concentration of diethylene glycol monobutyl ether in the leavening agent prepared according to the present invention is less than 30g/L, the degumming rate is less than 0.16mg/cm2The glue removing rate is low, and the risk of incomplete glue removing exists; when the concentration of the diethylene glycol monobutyl ether is 40-80g/L, the degumming speed is 0.28-0.34mg/cm2And the glue removal is normal. Based on cost consideration, the optimal concentration of the diethylene glycol monobutyl ether in the leavening agent is 40-50 g/L.
3. Chemical copper deposition backlight test of swelling agent on plates with different TG values
A plurality of test holes are drilled in the boards with different TG values, a multilayer printed circuit test board of FR4 board with the hole diameter of 0.1mm-1.0mm and the board thickness of 1.6mm +/-0.16 mm is processed according to the traditional hole metallization process flow, the leavening agent prepared in the embodiment 1 is adopted as the leavening agent, and the processed test board is subjected to hole metallization performance backlight test. Backlight rating by conventional backlight test method: slicing, grinding the hole to a half, observing under a metallographic microscope, lighting the slice from bottom to top under the slice by using a 25W bulb, observing the slice from top to bottom by an observer, judging the brightness avoidance degree of the hole wall by using a backlight grade chart, grading the backlight grade to 1-10, wherein the backlight grade chart of the circuit board is shown in figure 1, and the higher the grade is, the better the hole metallization is, and the better the backlight performance is. The backlight test results are shown in table 11.
Table 11: example 1 results of electroless copper plating backlight test of leavening agent on different TG value boards
Item | TG value of 140 deg.C | TG value of 160 ℃ C | TG value of 180 deg.C |
Backlight grade with aperture of 0.1 |
10 | 9.5 | 9 |
Backlight grade with aperture of 0.3 |
10 | 9.5 | 9 |
Backlight grade with aperture of 0.5 |
10 | 9.5 | 9.5 |
Backlight grade with aperture of 0.7 |
10 | 9.5 | 9 |
Backlight grade with aperture of 0.9mm | 9.5 | 9.5 | 9 |
The test results in Table 11 show that the leavening agent prepared by the invention has excellent hole metallization effect (backlight grade is more than 9) on micro holes (0.1mm-0.9mm) in a multilayer printed circuit board with medium and high TG value (TG value 140-.
The above examples are preferred embodiments of the present invention, but the present invention is not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and they are included in the scope of the present invention.
Claims (10)
1. A leavening agent, which is characterized in that: the leavening agent comprises the following components: monobutyl ether derivative, butanediol, phosphoric acid and water.
2. The leavening agent of claim 1, wherein: the monobutyl ether derivative comprises at least one of diethylene glycol monobutyl ether, triethylene glycol monobutyl ether, ethylene glycol monobutyl ether and dipropylene glycol monobutyl ether.
3. The leavening agent according to claim 1 or 2, characterized in that: the mass concentration of each component is as follows:
5 g/L-120 g/L of monobutyl ether derivative;
5 g/L-30 g/L of butanediol;
1 g/L-6 g/L phosphoric acid.
4. The leavening agent according to any one of claims 1 to 3, characterized in that: the degumming speed of the leavening agent is 0.15mg/cm2-0.45mg/cm2。
5. A process for preparing a leavening agent as claimed in any one of claims 1 to 4, wherein: the method comprises the following steps:
and mixing the components to obtain the leavening agent.
6. Use of the leavening agent of any one of claims 1 to 4 for removing circuit board smear.
7. Use according to claim 6, characterized in that: the glass transition temperature of the circuit board is 140-180 ℃.
8. Use according to claim 6, characterized in that: the diameter of the drilled hole with the drilling dirt is 0.08mm-1.2mm, and the depth of the drilled hole is 1.2mm-2.0 mm.
9. A method for removing circuit board drilling dirt is characterized in that: the method comprises the following steps:
cleaning the circuit board by immersing the circuit board in the swelling agent according to any one of claims 1 to 4.
10. The method of claim 9, wherein: the immersion temperature is 50-80 ℃, and the immersion time is 4-12 min.
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CN112969304A (en) * | 2021-02-04 | 2021-06-15 | 深圳中科利尔科技有限公司 | Swelling agent and method for removing residues in holes of circuit board |
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 |
CN113980753A (en) * | 2021-10-26 | 2022-01-28 | 江西超洋科技有限公司 | Novel leavening agent and preparation method thereof |
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JP2002246730A (en) * | 2001-02-13 | 2002-08-30 | Mitsubishi Electric Corp | Method and system for desmearing printed wiring board |
TW200712105A (en) * | 2005-09-30 | 2007-04-01 | Taiwan Uyemura Co Ltd | The leavening agent |
CN107278053A (en) * | 2016-04-08 | 2017-10-20 | 东莞市斯坦得电子材料有限公司 | The bulk softening process of the leading through-hole wall epoxy resin of hole metallization is turned on for printed wiring board |
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