CN116574565B

CN116574565B - Soldering flux cleaning agent for chip packaging, preparation method and application thereof

Info

Publication number: CN116574565B
Application number: CN202310445097.6A
Authority: CN
Inventors: 侯军; 隋新; 任浩楠; 吕晶
Original assignee: Dalian Aufirst Technology Co ltd
Current assignee: Dalian Aufirst Technology Co ltd
Priority date: 2023-04-24
Filing date: 2023-04-24
Publication date: 2024-04-16
Anticipated expiration: 2043-04-24
Also published as: CN116574565A

Abstract

The invention provides a scaling powder cleaning agent for chip packaging, a preparation method and application thereof. The invention relates to a scaling powder cleaning agent, which comprises the following components in parts by weight: 0.01-0.1 part of active enzyme; 0.1-1.5 parts of stabilizer; 10-25 parts of aprotic solvent; 5-20 parts of wetting agent; 10-40 parts of polar organic solvent; alcohol amine 5-25 parts; 45-60 parts of ultrapure water. The active enzyme is one or more selected from protease, lipase and cellulase. The invention also discloses a preparation method of the scaling powder cleaning agent and application of the scaling powder cleaning agent in the field of scaling powder cleaning. The scaling powder cleaning agent is safe, environment-friendly and efficient, does not corrode the metal surface, and can maintain extremely excellent cleaning efficiency under the pure soaking process condition of cleaning without matching an ultrasonic process.

Description

Soldering flux cleaning agent for chip packaging, preparation method and application thereof

Technical Field

The invention relates to a cleaning agent technology, in particular to a scaling powder cleaning agent for chip packaging, a preparation method and application thereof.

Background

The traditional detergent containing ODS substances such as freon has stronger dissolving capacity to grease rosin and other resins, has high efficiency and good stability, has no corrosiveness to metal materials and does not damage cleaned components, so the detergent is widely applied to cleaning of electronic industry products in early stage, but contains substances which damage ozone layers, and is harmful to the environment and human bodies in the production process, such as hydrochlorofluorocarbon, perfluorocarbon and other halogenated hydrocarbon detergents.

At present, a large amount of solvent type cleaning agents are used in the precision cleaning industry, mainly comprising petroleum type, alcohols, ethers, glycol esters, siloxanes, pyrrolidone and the like, but the solvent type cleaning agents have the defects of high price, high toxicity, high volatility, inflammability, explosiveness, unsafe operation and the like, and in addition, the whitening phenomenon of the cleaned surface of the low-carbon alcohol can occur due to the high water absorption.

The CN102051286B patent discloses a water-based cleaning agent for rosin type solder paste, which comprises 5wt% of diethylene glycol monomethyl ether, 15wt% of ethylene glycol monobutyl ether, 20wt% of 1, 2-propylene glycol diethyl ether, 1wt% of monoethanolamine, 0.1wt% of sodium perfluorononoxybenzene sulfonate, 0.01wt% of cyclohexylamine and the balance of water. The solvent of the cleaning agent contains alcohol ether organic matters, wherein diethylene glycol monomethyl ether, ethylene glycol monobutyl ether and propylene glycol diethyl ether are easy to burn to cause fire, and in the preparation process of the cleaning agent, especially ethylene glycol monobutyl ether can inhibit central nerves, high concentration can cause dizziness, nausea and other phenomena, and extremely high concentration can cause consciousness loss and even death. The other two ether substances also have toxicity and harm to human health.

CN102851151a discloses an environment-friendly cleaning agent for electronic industry, which comprises 2-methylpentane, absolute ethyl alcohol and an ether solvent, wherein methylpentane is used for replacing normal hexane, so that toxicity of the cleaning agent to human body is reduced, the cleaning agent has good solubility to rosin in soldering flux, the ether solvent has good solubility to organic acid in soldering flux, and the absolute ethyl alcohol has good greasy dirt removing effect, but the prepared cleaning agent is still toxic to human body, does not contain moisture, and is easy to cause pollution and residue to cleaning devices, so that secondary pollution is caused.

At present, most of the existing water-based cleaning agents are weak alkaline, contain inorganic salts and inorganic bases, cause certain corrosion to integrated chips, and increase the cost of the cleaning agents, so that the development of the water-based scaling powder cleaning agent with excellent corrosion inhibition performance for chip packaging is very necessary.

Disclosure of Invention

The invention aims to solve the problems that the existing water-based cleaning agent corrodes an integrated chip and the cleaning agent has high cost, and provides a scaling powder cleaning agent for chip packaging, which is safe, environment-friendly and efficient, does not corrode the metal surface, and can maintain extremely excellent cleaning efficiency under the pure soaking process condition of cleaning without matching an ultrasonic process.

It should be noted that, in the present invention, unless otherwise specified, reference to the specific meaning of "comprising" as defined and described by the composition includes both the open meaning of "comprising", "including" and the like, and the closed meaning of "consisting of …" and the like.

In order to achieve the above purpose, the invention adopts the following technical scheme: the soldering flux cleaning agent for chip packaging comprises the following components in parts by weight:

further, the active enzyme is selected from one or more of protease, lipase and cellulase.

Further, the active enzyme is preferably lipase.

Further, the lipase is selected from lipases with enzyme activities of 10 ten thousand to 40 ten thousand.

Further, the lipase preferably has an enzyme activity of 15 ten thousand to 25 ten thousand.

Further, the lipase is more preferably a lipase having an enzyme activity of 20 ten thousand.

Further, the active enzyme is 0.01-0.05 part.

Further, the stabilizer is one or more selected from pentaerythritol, glycerol, trimethylolethane, xylitol, sorbitol, 1, 4-butanediol, 1, 6-hexanediol, neopentyl glycol, diethylene glycol, dipropylene glycol and trimethylolpropane.

Further, the stabilizer is preferably sorbitol.

Further, the stabilizer is 0.5-1 part.

Further, the weight ratio of the active enzyme to the stabilizer is 1:10-30. At this ratio, the stabilizer stabilizes the active enzyme to maintain its activity and exert a good cleaning ability.

Further, the weight ratio of the active enzyme to the stabilizer is preferably 1:15-25.

Further, the weight ratio of the active enzyme to the stabilizer is more preferably 1:20.

Further, the aprotic solvents are otherwise referred to as aprotic solvents, and the proton self-transfer reaction of such solvents is extremely weak or has no tendency to self-transfer. The aprotic solvent is selected from one or more of acetonitrile, dimethylformamide, hexamethylphosphoric triamide and 1, 3-dimethyl-2-imidazolidinone (DMI).

Further, the aprotic solvent is preferably 1, 3-dimethyl-2-imidazolidinone.

Further, the aprotic solvent is 10-15 parts.

Further, the wetting agent is one or more of a glycoside surfactant, a glycoside surfactant derivative and a nonionic surfactant.

Further, the wetting agent is selected from one or more of N-dodecyl-N-methyl glucamide (MGEA-12), sodium glycosylsulfosuccinate, C8-16 Alkyl Polyglycoside (APG), alkyl polyglycoside sulfate, alkyl polyglycoside sulfosuccinate disodium salt (APG-SS), alkyl polyglycoside citrate disodium salt (APG-EC), alkyl polyglycoside tartrate disodium salt (APG-ET), alkyl polyglycoside phosphate and carboxymethyl alkyl polyglycoside.

Further, the wetting agent is preferably N-dodecyl-N-methyl glucamide (MGEA-12) and/or C8-16 Alkyl Polyglycoside (APG).

Further, the wetting agent is more preferably C8-12 Alkyl Polyglycoside (APG).

Further, the wetting agent is 5-10 parts.

Further, the weight ratio of the aprotic solvent to the wetting agent is 1:2-5:1. Under the proportion, the aprotic solvent and the wetting agent have good synergistic effect, so that the cleaning capability can be enhanced, and the corrosion of the cleaning agent on metals can be reduced;

further, the weight ratio of the aprotic solvent to the wetting agent is preferably 1:2 to 2:1.

Further, the weight ratio of the aprotic solvent to the wetting agent is more preferably 1:1.

Further, the polar organic solvent is selected from sulfone polar organic solvents and/or alcohol polar organic solvents.

Further, the sulfone polar organic solvent is selected from one or more of dimethyl sulfone, dimethyl sulfoxide, diethyl sulfone, n-propyl sulfone and sulfolane.

Further, the sulfone-based polar organic solvent is preferably dimethyl sulfoxide.

Further, the alcohol polar organic solvent is selected from one or more of methanol, ethanol, propanol, propylene glycol, 1,2 propylene glycol, tetrahydrofurfuryl alcohol and benzyl alcohol.

Further, the alcohol-based polar organic solvent is preferably 1, 2-propanediol.

Further, the polar organic solvent is 10-15 parts.

Further, the alcohol amine is selected from one or more of monoethanolamine, diethanolamine, triethanolamine, diglycolamine and isopropanolamine.

Further, the alcohol amine is preferably isopropanolamine.

Further, the alcohol amine is 10-20 parts.

Further, the ultrapure water is deionized water with the resistance of more than or equal to 18MΩ.

Further, the ultrapure water is 45-55 parts.

The scaling powder cleaning agent has the dual functions of corrosion inhibition and emulsion stability, the corrosion inhibition function can protect a substrate from corrosion, and the emulsion stability function is a surfactant in the system, so that the uniform oil-water mixing of the whole system is ensured, and the emulsion with good storage performance is obtained.

The invention also discloses a preparation method of the soldering flux cleaning agent for chip packaging, which comprises the following steps:

step (1): adding an aprotic solvent, a wetting agent, a stabilizer and active enzyme into a stirring kettle, and stirring to obtain a clear and transparent solution;

step (2): adding a polar organic solvent, alcohol amine and ultrapure water into the solution obtained in the step (1), and uniformly stirring and mixing to obtain a scaling powder cleaning agent;

the invention also discloses application of the soldering flux cleaning agent for chip packaging in the field of chip packaging soldering flux cleaning.

Further, the scaling powder cleaning agent is adopted to clean scaling powder, and the scaling powder cleaning agent is a pure soaking process without matching with an ultrasonic process for cleaning.

Further, the step of cleaning the chip with the soldering flux by using the soldering flux cleaning agent is as follows:

step (1): soaking the chip with the soldering flux in a soldering flux cleaning agent at 50-80 ℃ for 60-240 minutes to obtain a soaked chip;

step (2): and (3) flushing the chips soaked in the step (1) twice by using ultrapure water to finish the cleaning of the chips.

Furthermore, the soaked chips can be completely removed by washing with pure water without using acetone for rinsing.

Further, the soaking temperature in the step (1) is 50-60 ℃.

Further, the soaking time in the step (1) is 60-120 minutes.

The soldering flux cleaning agent for chip packaging prepared by the invention has the advantages of simple action mechanism, good stability, no layering after long-time storage and more convenient use. The scaling powder cleaning agent provided by the invention is safe, environment-friendly and efficient, and has the following advantages of no corrosion to the metal surface:

1. the scaling powder cleaning agent for chip encapsulation adopts the combination of a wetting agent and active enzyme, such as a coating or a lipid coating formed by wetting agent C8-16 alkyl polyglycoside APG and lipase, the active enzyme is immobilized to prevent the inactivation of the active enzyme, so that the active enzyme shows higher activity and stability in the cleaning agent, and meanwhile, the system can increase the dispersity of the lipase in an organic medium, thereby improving the reactivity of the enzyme, avoiding the direct contact of the active enzyme with a solvent, ensuring that the active enzyme wrapped by the surfactant has better stability, and further improving the cleaning capability of the cleaning agent.

2. The soldering flux cleaning agent for chip packaging can further stabilize active enzyme by adding a specific stabilizer, so that the active enzyme can keep activity and has good cleaning capability.

3. The scaling powder cleaning agent for chip packaging is added with the aprotic solvent, such as DMI, and the solution prepared by using the scaling powder cleaning agent has the characteristics of low viscosity, strong permeability, high boiling point and high temperature resistance, has good synergistic effect with a wetting agent, can enhance the cleaning capability, and can reduce the corrosion of the cleaning agent on metals; meanwhile, the glucoside wetting agent has more excellent wetting effect, can effectively act on surfaces which are difficult to wet, such as blind holes, gaps and the like, and remarkably improves the cleaning effect.

4. The soldering flux cleaning agent for chip packaging adopts various organic solvents and alcohol amine, has good dissolving and removing capacity for organic acid, organic amine, rosin, gum and other substances, and has good low-temperature cleaning effect.

5. The scaling powder cleaning agent for chip packaging has no problems of volatilization, inflammability, explosiveness and the like, does not need to use acetone for rinsing after cleaning, can be completely removed by only using pure water for rinsing, and has no harm to the environment and human body.

In summary, the soldering flux cleaning agent for chip packaging has no harm to human health, is safe, convenient and nontoxic to use, and has a simple and convenient use method. Therefore, the cleaning agent provided by the invention has very good application prospect and large-scale industrialized popularization potential in the field of semiconductor chip cleaning.

Drawings

Fig. 1 is a microscopic image of the rear surface of a chip with flux washed using example 1 at 20 x magnification.

Fig. 2 is a microscopic image of the rear surface of the chip after cleaning with the flux using comparative example 1 at 20 x magnification.

Detailed Description

The invention is further illustrated by the following examples:

examples 1 to 12

The example discloses a plurality of soldering flux cleaning agents for chip packaging, which comprise the following components in parts by weight as shown in table 1:

step (2): adding a polar organic solvent, alcohol amine and ultrapure water into the solution obtained in the step (1), and uniformly stirring and mixing to obtain the soldering flux cleaning agent for chip packaging.

Table 1 examples 1-12 compositions and weight ratios of the flux cleaner for chip packaging

Comparative examples 1 to 4

Comparative examples 1 to 4 disclose various flux cleaning solutions for chip packaging, which contain the components and weight ratios shown in table 2, and the preparation method thereof is the same as example 1.

Table 2 comparative examples 1-4 components and weight ratios of the flux cleaning liquid for chip packaging

Performance testing and description

The various properties of each of the above examples or comparative examples were tested below, and the surface cleaning was observed by using a microscope, and the corrosion rate was determined by measuring the concentrations of Cu and Sn ions by ICP-MS. The specific test results are shown in table 3: the chip with the soldering flux is cleaned by using the embodiments 1-12, no soldering flux remains on the surface of the cleaned chip, and the corrosion rate to Cu and Sn is low, which indicates that the chip has better protection effect; and the chip with the soldering flux is cleaned by adopting the comparative examples 1-4, a small amount of soldering flux and even a large amount of soldering flux still remain on the surface of the cleaned chip, and the corrosion rate to Cu and Sn is far higher than that of the examples 1-12, so that the chip is greatly damaged, and the yield of the chip is reduced.

TABLE 3 Performance test results

Fig. 1 is a microscopic image of the rear surface of a chip with flux washed using example 1 at 20 x magnification, and it can be seen from fig. 1 that the flux on the chip surface was washed clean with no residual flux using the chip with flux washed using example 1. Fig. 2 is a microscopic image of the rear surface of the chip with flux washed with comparative example 1 at 20 times magnification, and it can be seen from fig. 2 that a large amount of residual flux remains on the chip surface after the chip with flux is washed with comparative example 1.

Wherein:

the test method of the cleaning effect of the performance 1 comprises the following steps:

after reflow soldering and wave soldering processes, a large amount of flux residues remain on the chip, and the chip with the flux is cleaned by using the cleaning agent of the embodiment and the comparative example, and the cleaning treatment method comprises the following steps:

step 1: soaking the chip with the soldering flux in a soldering flux cleaning agent at 50 ℃ for 60 minutes to obtain a soaked chip;

step 2: placing the chip soaked in the step 1 into ultrapure water to be washed twice, thus finishing the cleaning of the chip;

step 3: and observing whether residual soldering flux exists on the surface of the cleaned chip by adopting an optical microscope.

Wherein, the ultrapure water used in the step 2 is deionized water with the resistance of at least 18MΩ.

The test method of the performance 2 metal corrosion rate comprises the following steps:

the ICP-MS method (inductively coupled plasma mass spectrometry) is adopted to test the corrosion performance of different cleaning agents on metals, and the specific test method is as follows: soaking 4×4cm chip with flux in cleaning agent at 85deg.C for 1 hr, measuring metal ion concentration in the cleaning agent by ICP-MS method, and calculating corrosion rateI.e. < ->May also be referred to as "etch rate") to examine the etch rate of different cleaners for metals.

Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.

Claims

1. The scaling powder cleaning agent for chip packaging is characterized by comprising the following components in parts by weight:

0.01-0.1 part of active enzyme;

0.1-1.5 parts of stabilizer;

10-25 parts of aprotic solvent;

5-20 parts of wetting agent;

10-40 parts of polar organic solvent;

alcohol amine 5-25 parts;

45-60 parts of ultrapure water;

the active enzyme is selected from one or more of protease, lipase and cellulase;

the stabilizer is one or more selected from pentaerythritol, glycerol, trimethylolethane, xylitol, sorbitol, 1, 4-butanediol, 1, 6-hexanediol, neopentyl glycol, diethylene glycol, dipropylene glycol and trimethylolpropane;

the wetting agent is selected from C8-16 alkyl polyglycosides;

the aprotic solvent is selected from one or more of acetonitrile, hexamethylphosphoric triamide and 1, 3-dimethyl-2-imidazolone;

the weight ratio of the aprotic solvent to the wetting agent is 1:2-5:1;

the weight ratio of the active enzyme to the stabilizer is 1:15-25;

the polar organic solvent is selected from sulfone polar organic solvents and/or alcohol polar organic solvents;

the alcohol amine is selected from one or more of monoethanolamine, diethanolamine, triethanolamine, diglycolamine and isopropanolamine.

2. A method for preparing the flux cleaner for chip packaging as claimed in claim 1, comprising the steps of:

step (2): adding a polar organic solvent, alcohol amine and ultrapure water into the solution obtained in the step (1), and uniformly stirring and mixing to obtain the scaling powder cleaning agent.

3. Use of the flux cleaner for chip package according to claim 1 for cleaning a chip package flux.

4. The use according to claim 3, wherein the flux cleaner for chip packaging is used to clean the flux using a pure immersion process without the need for ultrasonic process co-cleaning.