CN114989898A - Grinding and polishing residue cleaning solution and preparation method and application thereof - Google Patents

Abstract

The invention belongs to the technical field of fine chemical industry, and specifically discloses a cleaning solution for grinding and polishing residues and a preparation method and application thereof. In the present invention, surfactant with branched structure, ultra-high molecular weight polyethylene glycol rinsing aid, dispersant, self-defoaming cleaning aid, functional aid and stabilizer are added to water, mixed uniformly, and filtered. A cleaning solution for abrasive polishing residues is obtained. The invention avoids the introduction of nitrogen and phosphorus elements, solves the problem of great harm to the environment, has the characteristics of green environmental protection, and also has excellent cleaning function; and the preparation method is simple, easy for large-scale batch production, and has a wide range of applications.

Description

A cleaning solution for grinding and polishing residues and its preparation method and application

technical field

The invention relates to the technical field of fine chemicals, in particular to a cleaning solution for grinding and polishing residues and a preparation method and application thereof.

Background technique

Chemical grinding and polishing is an advanced technology for surface flattening in the process of large-scale advanced material or device manufacturing. It organically combines mechanical grinding and chemical reaction to achieve ultra-precision non-destructive surface processing. It is used in aviation, aerospace, microelectronics, It has been widely used in many fields such as integrated circuit manufacturing. Grinding and polishing slurries usually consist of components such as deionized water, oily ester solvents, abrasives, pH adjusters, oxidants, and dispersants. Abrasives play a role in grinding. Commonly used abrasives are silicon oxide, silicon carbide, boron carbide, diamond, iron oxide, chromium oxide and cerium oxide.

Improper cleaning of surface residues after grinding and polishing will lead to lower product qualification rates. Defective products caused by unclean surface residues can account for more than 50% of the total defective products. It can be seen that the level of cleaning quality has seriously affected the quality of the product. Performance, reliability and stability. In addition to the residual functional components after grinding and polishing, the ground powder also adheres to the surface or is squeezed into the shallow surface layer, which needs to be thoroughly cleaned. Cleaning liquid cleaning is to carry out physical and chemical action with the residue, so that the pollutants are dissolved in the cleaning liquid and detached from the surface of the substrate, or the bonding between the pollutants and the surface of the substrate is destroyed and detached.

Commercial cleaning solutions and public information in the industry show that existing cleaning solutions usually contain components such as organic bases, ethylenediaminetetraacetic acid and phosphates, polyvinylpolyamines, alkyl phosphates or nitrogen-containing cationic surfactants. To achieve the purpose of cleaning residues after grinding and polishing. This kind of cleaning liquid is rich in nitrogen and phosphorus elements, and the discharge of wastewater will aggravate the eutrophication and cyanobacteria of the water body and pollute the environment.

Therefore, how to provide a cleaning solution for grinding and polishing residues, and a preparation method and application thereof, so as to improve the cleaning effect, avoid the introduction of nitrogen and phosphorus elements, and improve the environmental protection performance of the cleaning solution is an urgent problem to be solved in the art.

SUMMARY OF THE INVENTION

In view of this, the present invention provides a cleaning solution for grinding and polishing residues and a preparation method and application thereof. The invention avoids the addition of components rich in nitrogen and phosphorus elements, strengthens the cleaning effect of the cleaning solution, and expands its application. scope.

In order to achieve the above object, the present invention adopts the following technical solutions:

A cleaning solution for grinding and polishing residues, comprising the following components in parts by mass: 0.5-5 parts of surfactant, 0.1-1 part of rinsing aid, 0.5-5 parts of dispersant, 5-10 parts of cleaning aid, functional 1-10 parts of auxiliary, 5-20 parts of stabilizer, 50-85 parts of water.

Preferably, the surfactant is a secondary alcohol polyoxyethylene ether and/or bis(1,3-dimethylbutanol) sulfosuccinate.

Preferably, the rinse aid is polyethylene glycol;

Wherein, the molecular weight of polyethylene glycol is 100,000 to 400,000 Daltons.

Preferably, the dispersant is tristyrylphenol polyoxypropylene polyoxyethylene block polymer and/or naphthol polyoxyethylene ether.

Preferably, the cleaning aid is a self-defoaming ether carboxylic acid.

Preferably, the functional auxiliary is one or more of acrylic acid and maleic acid polymer salt, carbonate, silicate and citrate;

Wherein, the molecular weight of the acrylic acid and maleic acid polymer salts is greater than or equal to 10,000 Daltons.

Preferably, the stabilizer is one or more of isoparaffin sulfate, ethylene glycol and propylene glycol.

Another object of the present invention is to provide a kind of preparation method of grinding and polishing residue cleaning liquid, and concrete preparation steps are as follows:

Mixing surfactant, rinsing aid, dispersing agent, cleaning aid, functional aid and stabilizer with water, and filtering to obtain a cleaning solution for grinding and polishing residues.

Another object of the present invention is to provide an application of a cleaning solution for grinding and polishing residues in the cleaning process of semiconductor silicon, sapphire, gallium arsenide, optical glass and metal devices.

The surfactant disclosed in the invention has a branched chain structure, can exhibit more excellent wetting and emulsifying properties, can promote the spreading of the cleaning solution on the cleaning interface, quickly wet the abrasive, and efficiently emulsify the oil-soluble medium. The cleaning aid has a short carbon-chain alkyl chain and a carboxyl structure, which can deeply clean the shallow surface of the interface and penetrate and peel off residues; in addition, its remarkable self-defoaming properties give the cleaning solution a remarkable feature of controllable foam, which is conducive to the control of the operation process . The functional additives can play the role of adjusting the pH value of the cleaning solution. The cleaning solution for grinding and polishing residues disclosed in the present invention is weakly acidic or neutral, which can prevent the cleaning solution from forming alkaline corrosion on the cleaned interface; silicate, carbonic acid Salts, citrates, and high molecular weight maleate and acrylic acid polymer salts can also bind metal ions and avoid ion residues. The stabilizer provides the storage stability of the cleaning solution under low temperature conditions or high temperature conditions, so that the cleaning solution is uniform and consistent, ensuring reliable and stable use. The dispersant of the invention has an electronic conjugated structure functional group structure, which is beneficial to avoid secondary pollution caused by the abrasives and organic macromolecules in the cleaning solution sticking back to the surface. Because the multi-branched surfactant has high surface activity and is easy to spread, it will increase the burden of rinsing after cleaning, and it is easy to cause the problem of unclean and residual rinsing. The ultra-high molecular weight polyethylene glycol rinse aid can improve the cleaning solution. Aqueous, significantly reducing the likelihood of potential carryover.

As can be seen from the above-mentioned technical solutions, compared with the prior art, the present invention has the following beneficial effects:

(1) The formula of the cleaning solution for grinding and polishing residues disclosed in the present invention is scientific and reasonable, avoids the introduction of nitrogen and phosphorus elements, is green and environmentally friendly, and also has excellent cleaning functions.

(2) The preparation method disclosed in the present invention is simple and easy to produce in large-scale batches.

(3) The cleaning solution for grinding and polishing residues disclosed in the present invention has a wide range of applications, can meet the cleaning of semiconductor silicon, sapphire, gallium arsenide, optical glass and metal devices and other materials, and will not be used in sensitive materials such as semiconductor silicon and gallium arsenide. Alkaline corrosion is formed on the surface.

Description of drawings

In order to explain the embodiments of the present invention or the technical solutions in the prior art more clearly, the following briefly introduces the accompanying drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only It is an embodiment of the present invention. For those of ordinary skill in the art, other drawings can also be obtained according to the provided drawings without creative work.

Fig. 1 is a result diagram of optical glass cleaning using the grinding and polishing residue cleaning solution prepared in Example 1;

Fig. 2 is the result diagram of optical glass cleaning with phosphorus-containing grinding cleaning solution;

FIG. 3 is a graph showing the results of cleaning optical glass with a nitrogen-containing non-foaming optical glass cleaning solution.

Detailed ways

The invention provides a cleaning solution for grinding and polishing residues, comprising the following components in parts by mass: 0.5-5 parts of surfactant, 0.1-1 part of rinsing aid, 0.5-5 parts of dispersant, and 5-5 parts of cleaning aid 10 parts, 1-10 parts of functional auxiliary, 5-20 parts of stabilizer, 50-85 parts of water; preferably 1-4 parts of surfactant, 0.3-0.8 parts of rinse aid, 2-4 parts of dispersant, cleaning 6-8 parts of auxiliary agent, 5-9 parts of functional auxiliary agent, 8-14 parts of stabilizer, 60-80 parts of water; more preferably 2 parts of surfactant, 0.5 part of rinse auxiliary, 3 parts of dispersant, cleaning auxiliary 7 parts of additives, 8 parts of functional additives, 10 parts of stabilizers, and 70 parts of water.

In the present invention, the surfactant is a surfactant with a branched chain structure, preferably a secondary alcohol polyoxyethylene ether and/or a bis(1,3-dimethylbutanol) sulfosuccinate salt, and further It is preferably a composition in which the mass ratio of one of Softanol-120/90/70/50/30 and AEROSOL MA 80 is 1:1.

In the present invention, the rinse aid is polyethylene glycol, and the molecular weight of polyethylene glycol is 100,000-400,000 Daltons, preferably 150,000-350,000 Daltons, and more preferably 300,000 Daltons.

In the present invention, the dispersant is a tristyryl phenol polyoxypropylene polyoxyethylene block polymer and/or a naphthol polyoxyethylene ether, preferably a naphthol polyoxyethylene ether Lugalvan BNO 12.

In the present invention, the cleaning aid is a self-defoaming ether carboxylic acid, preferably AKYPO LF2.

In the present invention, the functional auxiliary agent is one or more of acrylic acid and maleic acid polymer salt, carbonate, silicate and citrate, preferably citrate, more preferably citric acid sodium.

Wherein, the molecular weight of the acrylic acid and maleic acid polymer salts is greater than or equal to 10,000 Daltons.

In the present invention, the stabilizer is one or more of isoparaffin sulfate, ethylene glycol and propylene glycol, preferably isoparaffin sulfate.

In the present invention, the water is preferably deionized water.

The present invention also provides a method for preparing a cleaning solution for grinding and polishing residues, and the specific preparation steps are as follows:

Mixing surfactant, rinsing aid, dispersing agent, cleaning aid, functional aid and stabilizer with water, and filtering to obtain a cleaning solution for grinding and polishing residues.

In the present invention, the filtering precision of the filtering step is preferably 0.3 μm.

The invention also provides the application of a cleaning solution for grinding and polishing residues in the cleaning process of semiconductor silicon, sapphire, gallium arsenide, optical glass and metal devices.

In the present invention, the grinding and polishing residue cleaning solution is preferably used after mixing the grinding and polishing residue cleaning solution with water in a mass ratio of 3-10:100, more preferably 4-8:100, and further Preferably 6:100.

In the present invention, the washing temperature is preferably 40-70°C, more preferably 50°C; the washing time is preferably 3-10 minutes, more preferably 2-8 minutes, and still more preferably 5 minutes.

In the present invention, ultrasonic assistance is also included in the washing process.

The technical solutions in the embodiments of the present invention will be described clearly and completely below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

Example 1

2 parts Softanol-120 surfactant, 2 parts AEROSOL MA 80 surfactant, 0.5 part ultra-high molecular weight polyethylene glycol (molecular weight 300,000 Daltons), 3 parts Lugalvan BNO 12 naphthol polyoxyethylene ether, 8 parts of AKYPO LF2 self-defoaming ether carboxylic acid, 6 parts of sodium silicate, 5 parts of ethylene glycol, and 5 parts of propylene glycol were added to 65 parts of deionized water, mixed evenly, and filtered with a precision of 0.3 μm to obtain a cleaning solution for grinding and polishing residues .

Example 2

3 parts of 15-S-9 surfactant, 0.1 part of ultra-high molecular weight polyethylene glycol (molecular weight of 100,000 Daltons), 5 parts of triphenylethylphenol polyoxypropylene polyoxyethylene block polymer (1601 #polyether), 5 parts of AKYPO LF2 self-defoaming ether carboxylic acid, 8 parts of sodium citrate, 5 parts of isoparaffin sodium sulfate (solvay BOS) were added to 50 parts of deionized water, mixed well and filtered with 0.3μm precision A cleaning solution for grinding and polishing residues is obtained.

Example 3

Combine 2 parts Softanol-90 surfactant, 3 parts AEROSOL MA 80 surfactant, 1 part ultra-high molecular weight polyethylene glycol (molecular weight 200,000 Daltons), 5 parts Lugalvan BNO 12 naphthol polyoxyethylene ether, 10 parts of AKYPO LF2 self-defoaming ether carboxylic acid, 10 parts of sodium citrate, and 20 parts of ethylene glycol were added to 85 parts of deionized water, mixed evenly, and filtered with a precision of 0.3 μm to obtain a cleaning solution for grinding and polishing residues.

Example 4

0.5 part of AEROSOL MA 80 surfactant, 0.1 part of ultra-high molecular weight polyethylene glycol (molecular weight of 400,000 Daltons), 0.5 part of LugalvanBNO 12 naphthol polyoxyethylene ether, 5 parts of AKYPO LF2 self-defoaming ether carboxyl Acid, 1 part of sodium citrate, and 5 parts of propylene glycol are added to 50 parts of deionized water, mixed evenly, and filtered with a precision of 0.3 μm to obtain a cleaning solution for grinding and polishing residues.

Experimental example 1

The optical glass was cleaned with the grinding and polishing residue cleaning solutions prepared in Examples 1 to 4, respectively. The cleaning results of the grinding and polishing residue cleaning solutions prepared in Example 1 are shown in Figure 1. It can be seen that the grinding and polishing residues of the present invention are used. The optical glass after cleaning with the organic cleaning solution has no residual grinding powder and oily medium (Fig. 2 shows the cleaning results with phosphorus-containing abrasive cleaning solution (produced by Sandaoke), and Fig. 3 shows the use of nitrogen-containing non-foaming Optical glass cleaning solution (manufactured by Sandaoke) cleaning results.

Ammonia nitrogen determination kit and ammonium molybdate spectrophotometry (GB 11893-89) were respectively used to conduct ammonia nitrogen test and total phosphorus test on the cleaning solutions of grinding and polishing residues prepared in Examples 1 to 4 of the present invention; nitrogen and phosphorus elements were not detected. .

The various embodiments in this specification are described in a progressive manner, and each embodiment focuses on the differences from other embodiments, and the same and similar parts between the various embodiments can be referred to each other.

The above description of the disclosed embodiments enables any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (9)

1. A cleaning solution for grinding and polishing residues, characterized in that it comprises the following components in parts by mass: 0.5 to 5 parts of surfactant, 0.1 to 1 part of rinsing aid, 0.5 to 5 parts of dispersant, and 0.5 to 5 parts of cleaning aid 5 to 10 parts, 1 to 10 parts of functional additives, 5 to 20 parts of stabilizer, and 50 to 85 parts of water. 2. a kind of grinding and polishing residue cleaning solution according to claim 1, is characterized in that, described surfactant is secondary alcohol polyoxyethylene ether and/or sulfosuccinic acid bis(1,3-dimethylbutyl) alcohol) ester salt. 3. a kind of grinding and polishing residue cleaning solution according to claim 2, is characterized in that, described rinsing aid is polyethylene glycol; Wherein, the molecular weight of polyethylene glycol is 100,000 to 400,000 Daltons. 4. a kind of grinding and polishing residue cleaning solution according to claim 3, is characterized in that, described dispersant is tristyryl phenol polyoxypropylene polyoxyethylene block polymer and/or naphthol polyoxyethylene ether. 5 . The cleaning solution for grinding and polishing residues according to claim 1 , wherein the cleaning aid is a self-defoaming ether carboxylic acid. 6 . 6. a kind of grinding and polishing residue cleaning solution according to claim 5, is characterized in that, described functional assistant is in acrylic acid and maleic acid polymer salt, carbonate, silicate and citrate one or more; Wherein, the molecular weight of the acrylic acid and maleic acid polymer salts is greater than or equal to 10,000 Daltons. 7 . The cleaning solution for grinding and polishing residues according to claim 6 , wherein the stabilizer is one or more of isoparaffin sulfate, ethylene glycol and propylene glycol. 8 . 8. The preparation method of a cleaning solution for grinding and polishing residues according to any one of claims 1 to 7, wherein the surfactant, rinse aid, dispersant, cleaning aid, functional aid, stabilizer The agent is mixed with water and filtered to obtain a cleaning solution for grinding and polishing residues. 9. Application of the cleaning solution for grinding and polishing residues according to any one of claims 1 to 7 in the cleaning process of semiconductor silicon, sapphire, gallium arsenide, optical glass and metal devices.

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