Environment-friendly chip cleaning agent and preparation method thereof

Abstract

The invention is suitable for the technical field of chip cleaning, and provides an environment-friendly chip cleaning agent and a preparation method thereof, the environment-friendly chip cleaning agent comprises the following raw materials by mass: 73.0-78.0% of ultrapure water, 7.0-9.0% of castor oil-based polycarboxylic acid, 5.0-8.0% of castor oil polyoxyethylene ether, 3.0-6.0% of dehydrated castor oil, 2.0-4.0% of N-propionyl-N-hexyl hexadecanoic acid alkyl ester, and 2.0-3.0% of a preservative. The selected raw materials are good in biodegradability, liquid generated after cleaning is easy to treat and discharge and harmless to the environment, and the cleaning agent is simple in preparation process, convenient to operate, free of heating, low in energy consumption, free of three wastes, safe and environmentally friendly. Besides, the chip cleaning agent is an oil-in-water type neutral water-based cleaning agent, a layer of oil film can be formed on the surface of the chip after the chip is cleaned, the anti-rust and anti-corrosion performance of the chip is enhanced, and the chip cleaning agent is safe and reliable to use and store.

Description

Technical Field

[0001] This application belongs to the technical field of chip cleaning, and particularly relates to an environmentally friendly chip cleaning agent and a preparation method thereof. Background Art

[0002] In the process of chip preparation, multiple processes such as grinding, polishing, etching, cutting, and welding are required. Pollutants such as polishing wax, metal particles, flux, and etching solution will remain on the chip surface. Therefore, the chip needs to be cleaned later to remove pollutants to ensure the high quality of the chip. However, the use of inappropriate cleaning agents will lead to the generation of a large number of defective chips with problems such as leakage, short circuit, corrosion, rust, and metal migration, causing serious economic losses. For example, the integrated circuit chip cleaning agent of the prior art uses citric acid, glycerol, ethanol, polyoxyethylene ether, hydrogen peroxide, ammonium hydroxide, butane, and alkylolamide as raw materials. Among them, ethanol is volatile and not conducive to long-term storage; ammonium hydroxide is volatile and emits ammonia gas, is alkaline, has corrosiveness and strong irritation, and is likely to cause corrosion of the chip and harm to human health; hydrogen peroxide is easy to decompose and is not conducive to long-term storage; and the semiconductor chip cleaning agent in the prior art uses emulsifier, protective agent, hydrofluoric acid, ammonium fluoride, organic solvent, and ultrapure water as raw materials. Among them, hydrofluoric acid has extremely strong corrosiveness and can strongly corrode metals, glass, and silicon-containing objects. Inhaling the vapor or contacting the skin will cause incurable burns; ammonium fluoride has corrosiveness and toxicity and is easily decomposed into NH 3 and HF, which are harmful to both the environment and human health.

[0003] Therefore, it is very necessary to develop an environmentally friendly chip cleaning agent that is non-corrosive, harmless to the environment and human health, and will not damage the chip. Summary of the Invention

[0004] The purpose of the embodiment of this application is to provide an environmentally friendly chip cleaning agent, aiming to solve the problems that the existing chip cleaning agents have strong corrosiveness, are harmful to the environment and human health, and are likely to damage the chip.

[0005] The embodiment of this application is implemented as follows. An environmentally friendly chip cleaning agent is characterized by including the following raw materials in mass percentage:

[0006] Ultrapure water 73.0 - 78.0 wt%, castor oil-based polycarboxylic acid 7.0 - 9.0 wt%, castor oil polyoxyethylene ether 5.0 - 8.0 wt%, dehydrated castor oil 3.0 - 6.0 wt%, N-propionyl-N-hexyl hexadecanoate 2.0 - 4.0 wt%, and preservative 2.0 - 3.0 wt%.

[0007] Another purpose of the embodiment of this application is a preparation method of the above-mentioned environmentally friendly chip cleaning agent, including:

[0008] Weigh each raw material according to the formula of the above-mentioned environmentally friendly chip cleaning agent;

[0009] Add ultrapure water, castor oil-based polycarboxylic acid, castor oil polyoxyethylene ether, dehydrated castor oil, N-propionyl-N-hexyl hexadecanoate and preservative into the reaction device in sequence. During the feeding process, continuously stir mechanically at a speed of 60 - 100 n / min. After all the materials are added, continue to stir mechanically at a speed of 60 - 100 n / min for 10 - 20 min at room temperature to obtain the environmentally friendly chip cleaning agent.

[0010] The environmentally friendly chip cleaning agent provided by the embodiment of the present application is obtained by mixing components such as castor oil-based polycarboxylic acid, castor oil polyoxyethylene ether, dehydrated castor oil, N-propionyl-N-hexyl hexadecanoate, etc. in a certain proportion. The selected raw materials have good biodegradability, the liquid generated after cleaning is easy to treat and discharge, is harmless to the environment, and its preparation process is simple, convenient to operate, does not require heating, has low energy consumption, does not generate three wastes, and is safe and environmentally friendly. In addition, this chip cleaning agent is an oil-in-water type and neutral water-based cleaning agent. After the chip is cleaned, an oil film can be formed on the surface, enhancing the rust prevention and corrosion resistance of the chip, and both use and storage are safe and reliable. Specific Embodiments

[0011] In order to make the purpose, technical solutions and advantages of the present application clearer, the following further details the present application with reference to embodiments. It should be understood that the specific embodiments described herein are only used to explain the present application and are not used to limit the present application.

[0012] The embodiment of the present application provides an environmentally friendly chip cleaning agent, which includes the following raw materials in mass percentage:

[0013] Ultrapure water 73.0 - 78.0 wt%, castor oil-based polycarboxylic acid 7.0 - 9.0 wt%, castor oil polyoxyethylene ether 5.0 - 8.0 wt%, dehydrated castor oil 3.0 - 6.0 wt%, N-propionyl-N-hexyl hexadecanoate 2.0 - 4.0 wt% and preservative 2.0 - 3.0 wt%.

[0014] Preferably, the environmentally friendly chip cleaning agent includes the following raw materials in mass percentage:

[0015] Ultrapure water 76 wt%, castor oil-based polycarboxylic acid 8.3 wt%, castor oil polyoxyethylene ether 5.9 wt%, dehydrated castor oil 3.5 wt%, N-propionyl-N-hexyl hexadecanoate 3.3 wt% and preservative 3.0 wt%.

[0016] In the embodiment of the present application, the castor oil-based polycarboxylic acid is prepared by free radical polymerization at 25 °C using methyl allyl polyoxyethylene ether, castor oil, and fumaric acid as monomers, thioglycolic acid as a chain transfer agent, and a hydrogen peroxide and ascorbic acid redox system as an initiator.

[0017] The castor oil-based polycarboxylic acid used in the following specific examples is prepared by free radical polymerization at 25 °C using methyl allyl polyoxyethylene ether (TPEG), castor oil (C.O), and fumaric acid (FA) as monomers, thioglycolic acid (TGA) as a chain transfer agent, and a hydrogen peroxide (H 2 O 2 ) and ascorbic acid (Vc) redox system as an initiator. Specifically, a certain amount of TPEG and FA are added to a four-necked flask and deionized water is added. After stirring until completely dissolved at 25 °C, H 2 O 2 and C.O are added to the four-necked flask. Under continuous stirring, a solution composed of Vc, TGA, and deionized water is continuously added dropwise using a peristaltic pump at a dropping rate of 0.3 mL / min for 1 h. After the dropping is completed, the reaction continues for 1 h under the conditions of constant stirring rate and temperature. After the reaction is completed, the pH value is adjusted to about 7 with 40% NaOH solution to obtain the castor oil-based polycarboxylic acid. Among them, the molar ratio of each substance is: n(TPEG):n(C.O):n(FA):n(H 2 O 2 ):n(Vc):n(TGA)=1:0.43:2.48:0.4:0.023:0.16.

[0018] In the embodiment of the present application, the dehydrated castor oil is prepared by catalytic dehydration of castor oil.

[0019] The dehydrated castor oil used in the following specific examples is prepared by catalytic dehydration of castor oil with H-Beta molecular sieve at 160-180 °C. Specifically, a certain amount of castor oil and H-Beta molecular sieve catalyst are added to a three-necked flask. The amount of H-Beta used is 1-2.5 wt% of the mass of castor oil. Nitrogen is introduced into the three-necked flask from the bottom through a gas pipe, and the water generated during the reaction is carried out by means of nitrogen. The reaction is stirred at 160-180 °C for 1-3 h; after the reaction is completed, the catalyst is removed by filtration to obtain the dehydrated castor oil.

[0020] In the embodiment of the present application, the alkyl group in the N-propionyl-N-hexyl hexadecanoate refers to a straight-chain alkyl group of C8-C12, and is specifically obtained by reacting α-chloroalkyl hexadecanoate with N-hexyl propionamide under the action of a nano nickel oxide-zirconia composite catalyst.

[0021] Specifically, when N-propionyl-N-hexyl hexadecanoate is N-propionyl-N-hexyl octadecylate, it is prepared by the following method: 1.83 g of nickel nitrate, 2.71 g of zirconium nitrate and 2.07 g of template N-octanoyl-N-butyldodecylammonium (the molar ratio of NiO, ZrO 2 and the template is 1:0.8:0.5) are ground and mixed for 45 min (the rotation speed of the grinder is 600 r / min) to obtain a solid-phase reaction mixture; the solid-phase reaction mixture is placed in a supercritical crystallization kettle, nitrogen is introduced, and the temperature is raised to 50 °C for crystallization reaction, the pressure in the kettle is 5 MPa, and the crystallization reaction time is 3 h to obtain a crystallization product; the crystallization product is cooled to room temperature and then calcined at 600 °C for 1 h to obtain a nano-nickel oxide-zirconium oxide composite catalyst. 12.09 g of octadecyl α-chloride and 5.42 g of N-hexyl propionamide are added to a reaction vessel, and their molar ratio is 1:1.15; then 0.175 g of the nano-nickel oxide-zirconium oxide composite catalyst is added, and the reaction is carried out at 70 °C for 3 h. After the reaction is completed, the nickel oxide-zirconium oxide composite catalyst is removed by filtration, the filtrate is allowed to stand and layer, and the lower layer liquid is taken out to obtain N-propionyl-N-hexyl octadecylate.

[0022] In the embodiments of the present application, the ultrapure water is deionized water with a resistivity ≥ 18 Ω·m.

[0023] In the embodiments of the present application, the preservative is cetyltrimethylammonium chloride.

[0024] In the embodiments of the present application, ultrapure water, castor oil polyoxyethylene ether, and preservative are all commercially available raw materials.

[0025] The embodiments of the present application also provide a preparation method of the above-mentioned environmentally friendly chip cleaning agent, including:

[0026] Weigh each raw material according to the formula of the above-mentioned environmentally friendly chip cleaning agent;

[0027] Add ultrapure water, castor oil-based polycarboxylic acid, castor oil polyoxyethylene ether, dehydrated castor oil, N-propionyl-N-hexyl hexadecanoate alkyl ester, and preservative to the reaction device in sequence. During the feeding process, continuously stir mechanically at a rotation speed of 60-100 n / min. After all the materials are added, continue to stir mechanically at a rotation speed of 60-100 n / min at room temperature for 10-20 min to obtain the environmentally friendly chip cleaning agent.

[0028] The following uses specific examples to describe the environmentally friendly chip cleaning agent and its preparation method in detail, as shown below. The experimental methods used in the following examples are all conventional methods unless otherwise specified; the materials, reagents, etc. used are all commercially available unless otherwise specified.

[0029] Example 1

[0030] Add 36.5 g of ultrapure water, 4.05 g of hydrophilic emulsifier castor oil-based polycarboxylic acid, 3.6 g of lipophilic emulsifier castor oil polyoxyethylene ether, 2.75 g of base oil dehydrated castor oil, 1.4 g of preservative cetyltrimethylammonium chloride, and 1.7 g of rust inhibitor N-propionyl-N-hexyl octadecyl hexanoate into a beaker in sequence. During the feeding process, continuously stir mechanically at a speed of 80 n / min. After all the materials are added, continue to stir mechanically at a speed of 80 n / min for 20 min at room temperature to obtain an environmentally friendly chip cleaning agent. Among them, the mass percentage contents of ultrapure water, hydrophilic emulsifier, lipophilic emulsifier, base oil, preservative, and rust inhibitor are 73.0 wt%, 8.1 wt%, 7.2 wt%, 5.5 wt%, 2.8 wt%, and 3.4 wt% respectively.

[0031] Example 2

[0032] Add 39 g of ultrapure water, 3.9 g of hydrophilic emulsifier castor oil-based polycarboxylic acid, 3.15 g of lipophilic emulsifier castor oil polyoxyethylene ether, 1.55 g of base oil dehydrated castor oil, 1.4 g of preservative cetyltrimethylammonium chloride, and 1.0 g of rust inhibitor N-propionyl-N-hexyl nonyl hexanoate into a beaker in sequence. During the feeding process, continuously stir mechanically at a speed of 60 n / min. After all the materials are added, continue to stir mechanically at a speed of 60 n / min for 10 min at room temperature to obtain an environmentally friendly chip cleaning agent. Among them, the mass percentage contents of ultrapure water, hydrophilic emulsifier, lipophilic emulsifier, base oil, preservative, and rust inhibitor are 78.0 wt%, 7.8 wt%, 6.3 wt%, 3.1 wt%, 2.8 wt%, and 2.0 wt% respectively.

[0033] Example 3

[0034] Add 38 g of ultrapure water, 4.15 g of hydrophilic emulsifier castor oil-based polycarboxylic acid, 2.95 g of lipophilic emulsifier castor oil polyoxyethylene ether, 1.75 g of base oil dehydrated castor oil, 1.5 g of preservative cetyltrimethylammonium chloride, and 1.65 g of rust inhibitor N-propionyl-N-hexyl lauryl hexanoate into a beaker in sequence. During the feeding process, continuously stir mechanically at a speed of 100 n / min. After all the materials are added, continue to stir mechanically at a speed of 100 n / min for 15 min at room temperature to obtain an environmentally friendly chip cleaning agent. Among them, the mass percentage contents of ultrapure water, hydrophilic emulsifier, lipophilic emulsifier, base oil, preservative, and rust inhibitor are 76 wt%, 8.3 wt%, 5.9 wt%, 3.5 wt%, 3.0 wt%, and 3.3 wt% respectively.

[0035] Example 4

[0036] Add 37 g of ultrapure water, 4.0 g of hydrophilic emulsifier castor oil-based polycarboxylic acid, 3.25 g of lipophilic emulsifier castor oil polyoxyethylene ether, 2.75 g of base oil dehydrated castor oil, 1.0 g of preservative cetyltrimethylammonium chloride, and 2.0 g of rust inhibitor N-propionyl-N-hexadecyl decanoate into a beaker in sequence. During the feeding process, continuously stir mechanically at a speed of 70 n / min. After all the materials are added, continue to stir mechanically at a speed of 70 n / min for 20 min at room temperature to obtain an environmentally friendly chip cleaning agent. Among them, the mass percentage contents of ultrapure water, hydrophilic emulsifier, lipophilic emulsifier, base oil, preservative, and rust inhibitor are 74.0 wt%, 8.0 wt%, 6.5 wt%, 5.5 wt%, 2.0 wt%, and 4.0 wt% respectively.

[0037] Example 5

[0038] Add 36.65 g of ultrapure water, 4.5 g of hydrophilic emulsifier castor oil-based polycarboxylic acid, 4.0 g of lipophilic emulsifier castor oil polyoxyethylene ether, 2.15 g of base oil dehydrated castor oil, 1.35 g of preservative cetyltrimethylammonium chloride, and 1.35 g of rust inhibitor N-propionyl-N-hexadecyl laurate into a beaker in sequence. During the feeding process, continuously stir mechanically at a speed of 90 n / min. After all the materials are added, continue to stir mechanically at a speed of 90 n / min for 20 min at room temperature to obtain an environmentally friendly chip cleaning agent. Among them, the mass percentage contents of ultrapure water, hydrophilic emulsifier, lipophilic emulsifier, base oil, preservative, and rust inhibitor are 73.3 wt%, 9.0 wt%, 8.0 wt%, 4.3 wt%, 2.7 wt%, and 2.7 wt% respectively.

[0039] Comparative Example 1

[0040] Replace the dehydrated castor oil in the base oil with castor oil: According to the mass percentage contents of each raw material in Example 3, the mass percentage contents of ultrapure water, hydrophilic emulsifier, lipophilic emulsifier, base oil, preservative, and rust inhibitor are 76 wt%, 8.3 wt%, 5.9 wt%, 3.5 wt%, 3.0 wt%, and 3.3 wt% respectively. Add 38 g of ultrapure water, 4.15 g of hydrophilic emulsifier castor oil-based polycarboxylic acid, 2.95 g of lipophilic emulsifier castor oil polyoxyethylene ether, 1.75 g of base oil castor oil, 1.5 g of preservative cetyltrimethylammonium chloride, and 1.65 g of rust inhibitor N-propionyl-N-hexadecyl laurate into a beaker in sequence. During the feeding process, continuously stir mechanically at a speed of 100 n / min. After all the materials are added, continue to stir mechanically at a speed of 100 n / min for 15 min at room temperature.

[0041] Comparative Example 2

[0042] Adjust the addition order of raw materials: According to the mass percentage content of each raw material in Example 3, the mass percentage contents of base oil, hydrophilic emulsifier, lipophilic emulsifier, ultrapure water, preservative and rust inhibitor are 3.5 wt%, 8.3 wt%, 5.9 wt%, 76 wt%, 3.0 wt% and 3.3 wt% respectively. Add 1.75 g of dehydrated castor oil as base oil, 4.15 g of castor oil-based polycarboxylic acid as hydrophilic emulsifier, 2.95 g of castor oil polyoxyethylene ether as lipophilic emulsifier, 38 g of ultrapure water, 1.5 g of cetyltrimethylammonium chloride as preservative and 1.65 g of N-propionyl-N-hexyl lauryl hexanoate as rust inhibitor into the beaker in sequence. During the feeding process, continuously stir mechanically at a speed of 100 n / min. After all the materials are added, continue to stir mechanically at a speed of 100 n / min for 15 min at room temperature.

[0043] Comparative Example 3

[0044] Replace the rust inhibitor N-propionyl-N-hexyl lauryl hexanoate with alkylolamide: According to the mass percentage content of each raw material in Example 3, the mass percentage contents of ultrapure water, hydrophilic emulsifier, lipophilic emulsifier, base oil, preservative and rust inhibitor are 76 wt%, 8.3 wt%, 5.9 wt%, 3.5 wt%, 3.0 wt% and 3.3 wt% respectively. Add 38 g of ultrapure water, 4.15 g of castor oil-based polycarboxylic acid as hydrophilic emulsifier, 2.95 g of castor oil polyoxyethylene ether as lipophilic emulsifier, 1.75 g of dehydrated castor oil as base oil, 1.5 g of cetyltrimethylammonium chloride as preservative and 1.65 g of alkylolamide as rust inhibitor into the beaker in sequence. During the feeding process, continuously stir mechanically at a speed of 100 n / min. After all the materials are added, continue to stir mechanically at a speed of 100 n / min for 15 min at room temperature.

[0045] Comparative Example 4

[0046] Replace the hydrophilic emulsifier castor oil-based polycarboxylic acid with β-nicotinamide mononucleotide: According to the mass percentage content of each raw material in Example 3, the mass percentage contents of ultrapure water, hydrophilic emulsifier, lipophilic emulsifier, base oil, preservative and rust inhibitor are 76 wt%, 8.3 wt%, 5.9 wt%, 3.5 wt%, 3.0 wt% and 3.3 wt% respectively. Add 38 g of ultrapure water, 4.15 g of β-nicotinamide mononucleotide as hydrophilic emulsifier, 2.95 g of castor oil polyoxyethylene ether as lipophilic emulsifier, 1.75 g of dehydrated castor oil as base oil, 1.5 g of cetyltrimethylammonium chloride as preservative and 1.65 g of N-propionyl-N-hexyl lauryl hexanoate as rust inhibitor into the beaker in sequence. During the feeding process, continuously stir mechanically at a speed of 100 n / min. After all the materials are added, continue to stir mechanically at a speed of 100 n / min for 15 min at room temperature.

[0047] Comparative Example 5

[0048] Replace the lipophilic emulsifier castor oil polyoxyethylene ether with ethylene glycol monoethyl ether: According to the mass percentage content of each raw material in Example 3, the mass percentage contents of ultrapure water, hydrophilic emulsifier, lipophilic emulsifier, base oil, preservative and rust inhibitor are 76 wt%, 8.3 wt%, 5.9 wt%, 3.5 wt%, 3.0 wt% and 3.3 wt% respectively. Add 38 g of ultrapure water, 4.15 g of hydrophilic emulsifier castor oil-based polycarboxylic acid, 2.95 g of lipophilic emulsifier ethylene glycol monoethyl ether, 1.75 g of base oil dehydrated castor oil, 1.5 g of preservative cetyltrimethylammonium chloride and 1.65 g of rust inhibitor N-propionyl-N-hexyl laurate into a beaker in sequence. During the feeding process, continuously stir mechanically at a speed of 100 n / min. After all the materials are added, continue to stir mechanically at a speed of 100 n / min for 15 min at room temperature.

[0049] Comparative Example 6

[0050] Increase the mass percentage content of the hydrophilic emulsifier to 9.5 wt%: The mass percentage contents of ultrapure water, hydrophilic emulsifier, lipophilic emulsifier, base oil, preservative and rust inhibitor are 74.8 wt%, 9.5 wt%, 5.9 wt%, 3.5 wt%, 3.0 wt% and 3.3 wt% respectively. Add 37.4 g of ultrapure water, 4.75 g of hydrophilic emulsifier castor oil-based polycarboxylic acid, 2.95 g of lipophilic emulsifier castor oil polyoxyethylene ether, 1.75 g of base oil dehydrated castor oil, 1.5 g of preservative cetyltrimethylammonium chloride and 1.65 g of rust inhibitor N-propionyl-N-hexyl laurate into a beaker in sequence. During the feeding process, continuously stir mechanically at a speed of 100 n / min. After all the materials are added, continue to stir mechanically at a speed of 100 n / min for 15 min at room temperature.

[0051] Comparative Example 7

[0052] Reduce the mass percentage content of the hydrophilic emulsifier to 6.0 wt%: The mass percentage contents of ultrapure water, hydrophilic emulsifier, lipophilic emulsifier, base oil, preservative and rust inhibitor are 77.3 wt%, 6.0 wt%, 5.9 wt%, 4.5 wt%, 3.0 wt% and 3.3 wt% respectively. Add 38.65 g of ultrapure water, 3.0 g of hydrophilic emulsifier castor oil-based polycarboxylic acid, 2.95 g of lipophilic emulsifier castor oil polyoxyethylene ether, 2.25 g of base oil dehydrated castor oil, 1.5 g of preservative cetyltrimethylammonium chloride and 1.65 g of rust inhibitor N-propionyl-N-hexyl laurate into a beaker in sequence. During the feeding process, continuously stir mechanically at a speed of 100 n / min. After all the materials are added, continue to stir mechanically at a speed of 100 n / min for 15 min at room temperature.

[0053] Comparative Example 8

[0054] Reduce the mass percentage content of the lipophilic emulsifier to 4.5 wt%: The mass percentage contents of ultrapure water, hydrophilic emulsifier, lipophilic emulsifier, base oil, preservative, and rust inhibitor are 76 wt%, 8.3 wt%, 4.5 wt%, 4.9 wt%, 3.0 wt%, and 3.3 wt% respectively. Add 38.0 g of ultrapure water, 4.15 g of hydrophilic emulsifier castor oil-based polycarboxylic acid, 2.25 g of lipophilic emulsifier castor oil polyoxyethylene ether, 2.45 g of base oil dehydrated castor oil, 1.5 g of preservative cetyltrimethylammonium chloride, and 1.65 g of rust inhibitor N-propionyl-N-hexyl lauric acid ester into a beaker in sequence. During the feeding process, continuously stir mechanically at a speed of 100 n / min. After all the materials are added, continue to stir mechanically at a speed of 100 n / min for 15 min at room temperature.

[0055] Comparative Example 9

[0056] Increase the mass percentage content of the lipophilic emulsifier to 8.5 wt%: The mass percentage contents of ultrapure water, hydrophilic emulsifier, lipophilic emulsifier, base oil, preservative, and rust inhibitor are 73.0 wt%, 7.3 wt%, 8.5 wt%, 4.9 wt%, 3.0 wt%, and 3.3 wt% respectively. Add 36.5 g of ultrapure water, 3.65 g of hydrophilic emulsifier castor oil-based polycarboxylic acid, 4.25 g of lipophilic emulsifier castor oil polyoxyethylene ether, 2.45 g of base oil dehydrated castor oil, 1.5 g of preservative cetyltrimethylammonium chloride, and 1.65 g of rust inhibitor N-propionyl-N-hexyl lauric acid ester into a beaker in sequence. During the feeding process, continuously stir mechanically at a speed of 100 n / min. After all the materials are added, continue to stir mechanically at a speed of 100 n / min for 15 min at room temperature.

[0057] Comparative Example 10

[0058] Do not add base oil, and the mass percentage contents of the remaining components are all within the component content range of this application: The mass percentage contents of ultrapure water, hydrophilic emulsifier, lipophilic emulsifier, preservative, and rust inhibitor are 77 wt%, 8.8 wt%, 7.4 wt%, 3.0 wt%, and 3.8 wt% respectively. Add 38.5 g of ultrapure water, 4.4 g of hydrophilic emulsifier castor oil-based polycarboxylic acid, 3.7 g of lipophilic emulsifier castor oil polyoxyethylene ether, 1.5 g of preservative cetyltrimethylammonium chloride, and 1.9 g of rust inhibitor N-propionyl-N-hexyl lauric acid ester into a beaker in sequence. During the feeding process, continuously stir mechanically at a speed of 100 n / min. After all the materials are added, continue to stir mechanically at a speed of 100 n / min for 15 min at room temperature.

[0059] The chip cleaning agents obtained from the above embodiments and comparative examples were subjected to performance tests. The performance test results are shown in Table 1 below.

[0060] Among them, the method for detecting the stability of the cleaning agent: Use a pipette to drop 100 mL of the chip cleaning agent into a 100 mL burette, and observe whether stratification occurs after standing for 24 h; if stratification occurs, calculate the volume percentage of the separated upper oil layer in 100 mL of the chip cleaning agent. The smaller this value is, the better the stability of the chip cleaning agent.

[0061] The anti-corruption performance of the cleaning agent was judged by visual inspection and smelling: Take 100 mL of the chip cleaning agent and add it to a 100 mL beaker, and place it open in the room for 30 days, and observe the changes in its color and smell.

[0062] The method for testing the decontamination performance of the cleaning agent: Prepare 7 groups of chips with the same size, measure the initial weight respectively, denoted as W1. A layer of 10 grams of dirt (the dirt is evenly mixed by 10 grams of polishing wax and 10 grams of flux) is coated on the chips, and after drying at 100 °C for 1 hour, measure the weight respectively, denoted as W2. Cleaning method: Weigh 500 grams of the chip cleaning agent in the examples and the comparative examples respectively and pour them into a micro ultrasonic cleaner, clean the 7 groups of chips respectively, ultrasonically clean for 3 minutes at room temperature, then rinse with ultrapure water for 2 minutes, and place them in an oven at 100 °C to dry for 30 minutes, and measure the weight respectively, denoted as W3. Calculate the decontamination rate: Decontamination rate = [(W2 - W3) / (W2 - W1)] × 100%. The larger this value is, the better the cleaning effect of the cleaning agent on the chips.

[0063] Corrosion rate: The contents of Si and Cu elements on the chips before and after cleaning were determined by ICP-MS characterization method. The smaller this value is, the less corrosive the cleaning solution is to the chips and the better the protective effect.

[0064] The method for detecting the rust prevention performance: Immerse all the chips in the chip cleaning agent, then take them out and place them in a constant temperature oven at 25 o °C, and observe the time required for rust spots to appear. The longer the time, the better its rust prevention performance.

[0065] Table 1

[0066]

[0067] In summary, as can be seen from the performance test results in Table 1, in Comparative Example 1, when the dehydrated castor oil in Example 3 was replaced with castor oil, the stability, anti-corruption performance, rust prevention performance, cleaning and protection effects on the chips of the prepared chip cleaning agent were all reduced. The main reason is that there are isolated double bonds in the molecular structure of castor oil, which are easily oxidized by oxygen in the air, breaking the balance among the components in the chip cleaning agent system, and thus reducing the performance of the cleaning agent. In the examples, dehydrated castor oil is used, which has conjugated double bonds in its molecular structure and lower energy. This structure makes the molecule more stable than the molecule containing isolated double bonds, less likely to be oxidized and deteriorated, and is conducive to the long-term storage of the prepared chip cleaning agent.

[0068] In Comparative Example 2, after changing the feeding order in Example 3, the performance of the prepared chip cleaning agent was significantly reduced. The main reason is that the feeding order will ultimately affect the type of the chip cleaning agent, namely "water-in-oil" or "oil-in-water". In the examples, water is added first, followed by hydrophilic and lipophilic emulsifiers, and then oil, so the prepared chip cleaning agent is a water-in-oil microemulsion; while in Comparative Example 2, oil is added first, followed by hydrophilic and lipophilic emulsifiers, and then water, resulting in an oil-in-water emulsion. The microemulsion system is more stable than the emulsion system. Therefore, the chip cleaning agent prepared in Comparative Example 2 is prone to stratification and demulsification, leading to a significant reduction in various performances.

[0069] In Comparative Examples 3, 4 and 5, when the rust inhibitor, hydrophilic and lipophilic emulsifiers were replaced with substances in the reported prior art respectively, the rust prevention performance decreased. This is because the synergistic effects among different raw materials are different; although the rust inhibitor changed in Comparative Example 3, the system did not stratify and the stability was not affected. The main reason is that the hydrophilic and lipophilic emulsifiers did not change, which is also one of the key innovations of the chip cleaning agent prepared in this application. The synergistic effect of the hydrophilic emulsifier ricinoleic acid-based polycarboxylic acid and the lipophilic emulsifier ricinoleic acid polyoxyethylene ether is the key factor to ensure the good stability of the cleaning agent.

[0070] In Comparative Examples 6, 7, 8 and 9, when the mass percentage content of the hydrophilic and lipophilic emulsifiers changed outside the preferred range, the prepared chip cleaning agent was prone to stratification, with poor stability and reduced rust prevention and anti-corrosion performances.

[0071] In Comparative Example 10, when the base oil was not added, the rust prevention and anti-corrosion performances of the prepared chip cleaning agent decreased. The main reason is that the base oil can form an oil film on the cleaned chip, and the oil film is beneficial to rust prevention and anti-corrosion. The presence of base oil in the system is also one of the key innovations of the chip cleaning agent prepared in this application.

[0072] The above-described embodiments merely represent several implementation manners of the present application. The description thereof is relatively specific and detailed, but it should not be construed as a limitation on the scope of the present application. It should be noted that for those of ordinary skill in the art, without departing from the concept of the present application, several modifications and improvements can still be made, and these all fall within the protection scope of the present application. Therefore, the protection scope of the present application shall be subject to the appended claims.

[0073] The foregoing is only a preferred embodiment of the present application and is not intended to limit the present application. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present application shall be included within the protection scope of the present application.

Claims

1. An environmentally friendly chip cleaning agent, characterized in that: The following raw materials are included in mass percentage: Ultrapure water 73.0-78.0wt%, castor oil-based polycarboxylic acid 7.0-9.0wt%, castor oil polyoxyethylene ether 5.0-8.0wt%, dehydrated castor oil 3.0-6.0wt%, N-propionyl-N-hexylhexadecanoate 2.0-4.0wt% and preservative 2.0-3.0wt%.

2. The environmentally friendly chip cleaning agent according to claim 1, characterized in that: The following raw materials are included in mass percentage: Ultrapure water 76wt%, castor oil-based polycarboxylic acid 8.3wt%, castor oil polyoxyethylene ether 5.9wt%, dehydrated castor oil 3.5wt%, N-propionyl-N-hexylhexadecanoate 3.3wt% and preservative 3.0wt%.

3. The environmentally friendly chip cleaning agent according to claim 1 or 2, characterized in that: The castor oil-based polycarboxylic acid is prepared by free radical polymerization at 25° C., with methyl allyl polyoxyethylene ether, castor oil and fumaric acid as monomers, thioglycolic acid as a chain transfer agent, and hydrogen peroxide and ascorbic acid redox system as initiators.

4. The environmentally friendly chip cleaning agent according to claim 1 or 2, characterized in that: The dehydrated castor oil is prepared by catalytic dehydration of castor oil.

5. The environmentally friendly chip cleaning agent according to claim 4, characterized in that: The dehydrated castor oil is prepared by catalytically dehydrating castor oil with H-Beta molecular sieve at 160-180° C., wherein the amount of H-Beta molecular sieve used is 1-2.5 wt % of the mass of castor oil.

6. The environmentally friendly chip cleaning agent according to claim 1 or 2, characterized in that: The alkyl group in the N-propionyl-N-hexylhexadecanoate refers to a C8-C12 straight-chain alkyl group.

7. The environmentally friendly chip cleaning agent according to claim 1 or 2, characterized in that: The N-propionyl-N-hexyl hexadecanoic acid alkyl ester is obtained by reacting α-chlorohexadecanoic acid alkyl ester and N-hexyl propionamide as raw materials under the action of a nano nickel oxide-zirconium oxide composite catalyst.

8. The environmentally friendly chip cleaning agent according to claim 1 or 2, characterized in that: The ultrapure water is deionized water with a resistivity of ≥18 Ω·m.

9. The environmentally friendly chip cleaning agent according to claim 1 or 2, characterized in that: The preservative is cetyltrimethylammonium chloride.

10. A method for preparing the environmentally friendly chip cleaning agent according to claim 1, characterized in that: include: Weigh the raw materials according to the formula of the environmentally friendly chip cleaning agent according to claim 1; Ultrapure water, castor oil-based polycarboxylic acid, castor oil polyoxyethylene ether, dehydrated castor oil, N-propionyl-N-hexylhexadecanoate and preservative are added to the reaction device in sequence. During the adding process, mechanical stirring is continued at a speed of 60-100 n / min. After all the materials are added, mechanical stirring is continued at a speed of 60-100 n / min for 10-20 min at room temperature to obtain an environmentally friendly chip cleaning agent.

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