CN116042099B - Grinding aid with high wettability, high dispersion, high suspension and easy cleaning, preparation method and application thereof, and grinding fluid containing grinding aid - Google Patents

Abstract

The present invention provides a high-wetting, high-dispersion, high-suspending, easy-to-clean grinding aid, a preparation method, a use, and a grinding liquid containing the same. The grinding aid of the present invention is compounded with a dispersant, an anti-settling agent, a charge repulsion agent, a wetting agent, a defoaming agent, and an amphiphilic solvent, and is mixed with soft and hard abrasives to obtain a grinding liquid. The grinding aid of the present invention has extremely high surface dynamic wetting and penetration capabilities, is not easy to generate foam, can quickly spread on the surface of gallium arsenide, and can quickly penetrate into the microcracks on the surface of gallium arsenide to form a splitting effect and improve grinding efficiency; at the same time, it has a good dispersing and anti-settling effect on the abrasive, avoids the agglomeration of different micropowders and grinding chips during the grinding process, can make different types of abrasives evenly distributed in the grinding liquid, and keep a suspended state for a long time. During grinding, gallium arsenide is subjected to uniform force, the grinding rate is fast, the surface roughness after grinding is low, the TTV is low, the flatness is good and there are no obvious scratches, it is easy to clean, and there is no impurity residue on the surface.

Description

A high-wetting, high-dispersion, high-suspending, easy-to-clean grinding aid, preparation method, use, and grinding fluid containing the same

Technical Field

The invention relates to grinding liquid technology, and in particular to a high-wetting, high-dispersion, high-suspending and easy-to-clean grinding aid, a preparation method, a use and a grinding liquid containing the same.

Background Art

Gallium arsenide (GaAs) is a second-generation semiconductor and is known as the "semiconductor aristocrat" for its high price. Gallium arsenide is internationally recognized as the most mature compound semiconductor material after "silicon". It has superior characteristics such as high frequency, high electron mobility, high output power, low noise and good linearity. It is one of the most important supporting materials for the optoelectronics and microelectronics industries. The second-generation semiconductors represented by gallium arsenide are widely used in the manufacture of high-frequency, high-speed, high-power, low-noise, high-temperature resistant, and radiation-resistant integrated circuits. It has developed into a key technology for "modern electronic information products" and "information highways". The 5G chip market is very good and the product is in short supply.

Gallium arsenide, as a type of compound semiconductor, has a production process similar to that of most compound semiconductors such as silicon carbide and indium phosphide, including polycrystalline synthesis, single crystal growth, and then cutting, edging, grinding, polishing, cleaning and other processes. The grinding process is crucial to the quality of gallium arsenide substrates. Due to the low hardness and high brittleness of gallium arsenide, high-hardness abrasives and large particles in grinding can easily cause scratches on the surface of gallium arsenide. The uneven force on gallium arsenide sheets during grinding increases the breakage rate and affects production capacity. A large number of nano-scale inorganic particles will be generated during the gallium arsenide grinding process. Due to the electrostatic effect, they are very easy to form agglomerations and precipitates, and adsorb on the abrasive surface, resulting in a decrease in removal rate and surface scratches, which seriously affects the processing efficiency and production yield of gallium arsenide.

Gallium arsenide grinding fluid is mainly composed of abrasives, deionized water and suspension aids. Abrasives mainly include aluminum oxide, silicon oxide, etc. The hardness of pure aluminum oxide abrasive is too high, the edges are sharp, and it is easy to scratch. Silicon oxide has low hardness and low grinding efficiency. At the same time, it is easy to break into nano powder particles during the grinding process, which are coated on the surface of aluminum oxide particles to form agglomerated particles and cause scratches. In view of the requirements of processing efficiency and processing quality in the gallium arsenide grinding process, it is necessary to develop a gallium arsenide grinding fluid that takes into account both processing efficiency and processing quality.

At present, some grinding liquids have been disclosed that can be used for grinding gallium arsenide, such as:

CN115039203A discloses a polishing liquid, which contains abrasive grains, at least one hydroxy acid component selected from the group consisting of hydroxy acids and their salts, and compound Z, wherein compound Z has a hydrocarbon group and a polyoxyalkylene group that can be substituted. The polishing liquid group can be stored in a first liquid and a second liquid, wherein the first liquid contains abrasive grains, and the second liquid contains a hydroxy acid component and compound Z. The flatness of the substrate after polishing is improved.

CN110914958A discloses a grinding method and a grinding composition. The first grinding liquid used in the first pre-grinding stage may contain abrasive grains A1, water-soluble polymer P1 and water. The second grinding liquid used in the second pre-grinding stage may contain abrasive grains A2, water-soluble polymer P2 and water. The third grinding liquid used in the third pre-grinding stage may contain abrasive grains A3, water-soluble polymer P3 and water. After grinding, a surface with high flatness and low defects can be effectively achieved.

As mentioned above, the prior art has disclosed a variety of polishing liquids (additives), but these polishing liquids (additives) have the following defects to varying degrees: single abrasives are hard and easy to scratch, have insufficient wettability, cannot spread quickly on the surface of gallium arsenide, resulting in high TTV after polishing, insufficient suspension, and rapid sedimentation of abrasives that reduces the rate, etc. The polishing liquids (additives) in the prior art currently have various defects and are difficult to meet the increasingly demanding polishing needs.

Therefore, there is an urgent need to develop a high-wetting, high-dispersion, high-suspending, and easy-to-clean grinding fluid for gallium arsenide grinding.

Summary of the invention

The purpose of the present invention is to provide a high-wetting, high-dispersing, high-suspending and easy-to-clean grinding aid in view of the problems of low wetting, low suspension, difficulty in cleaning and insufficient dispersibility of existing grinding aids. The grinding aid has extremely high surface dynamic wetting and penetration ability, is not easy to generate foam, can quickly spread on the surface of gallium arsenide, and can quickly penetrate into the micro cracks on the surface of gallium arsenide to form a splitting effect and improve the grinding efficiency; at the same time, it has a good dispersing and anti-settling effect on abrasives, avoids the agglomeration of different micropowders and grinding chips during the grinding process, can make different types of abrasives evenly distributed in the grinding liquid, keep a suspended state for a long time, gallium arsenide is evenly stressed during grinding, the grinding rate is fast, the surface roughness after grinding is low, the TTV is low, the flatness is good, there are no obvious scratches, and it is easy to clean, and there is no impurity residue on the surface.

To achieve the above object, the technical solution adopted by the present invention is: a high-wetting, high-dispersibility, high-suspendability, and easy-to-clean grinding aid, comprising the following components in weight proportions:

Furthermore, the dispersant is one or more of maleic acid-acrylic acid copolymer, maleic acid-olefin copolymer, polyvinyl pyrrolidone-vinylimidazole copolymer, maleic acid-acrylic acid homopolymer and polyethyleneimine polyoxyethylene ether.

Furthermore, the dispersant is preferably polyethyleneimine polyoxyethylene ether.

Furthermore, the molecular weight of the maleic acid-acrylic acid copolymer is 50,000-70,000.

Furthermore, the molecular weight of the maleic acid-acrylic acid copolymer is preferably 50,000-60,000.

Furthermore, the molecular weight of the maleic acid-olefin copolymer is 5000-10000.

Furthermore, the molecular weight of the maleic acid-olefin copolymer is preferably 5000-8000.

Furthermore, the molecular weight of the polyvinyl pyrrolidone-vinylimidazole copolymer is 5000-20000.

Furthermore, the molecular weight of the polyvinyl pyrrolidone-vinylimidazole copolymer is preferably 5000-10000.

Furthermore, the molecular weight of the maleic acid-acrylic acid homopolymer is 3000-10000.

Furthermore, the molecular weight of the maleic acid-acrylic acid homopolymer is preferably 6000-9000.

Furthermore, the molecular weight of the polyethyleneimine polyoxyethylene ether is 30,000-60,000.

Furthermore, the molecular weight of the polyethyleneimine polyoxyethylene ether is preferably 40,000-50,000.

Furthermore, the dispersant is 1-3 parts.

Furthermore, the anti-settling agent is one or more of hydroxyethyl cellulose, alkali-swellable polyurethane, alkali-swellable acrylic polymer and polyvinyl alcohol.

Furthermore, the anti-settling agent is preferably an alkali-swellable acrylic polymer.

Furthermore, the molecular weight of the hydroxyethyl cellulose is 10,000-100,000.

Furthermore, the molecular weight of the hydroxyethyl cellulose is preferably 50,000-100,000.

Furthermore, the molecular weight of the alkali-swellable polyurethane is 3000-10000.

Furthermore, the molecular weight of the alkali-swellable polyurethane is preferably 3000-6000.

Furthermore, the molecular weight of the alkali-swellable acrylic polymer is 3,000-10,000.

Furthermore, the molecular weight of the alkali-swellable acrylic polymer is preferably 3000-5000.

Furthermore, the molecular weight of the polyvinyl alcohol is 50,000-200,000.

Furthermore, the molecular weight of the polyvinyl alcohol is preferably 50,000-100,000.

Furthermore, the anti-settling agent is 0.1-1 part.

Furthermore, the charge repulsive agent is a cationic complexing agent containing a polyamino structure.

Furthermore, the charge repulsive agent is one or more of diethylenetriamine, triethylenetetramine, triethylenetetramine, tetraethylenepentamine, DL-aminopropylene glycol, aminopentanol, N-(3-aminopropyl)diethanolamine, dicyclohexylamine, isopropanolamine and diglycolamine.

Furthermore, the charge repulsive agent is preferably triethylenetetramine.

Furthermore, the charge repulsion agent is 1-3 parts.

Furthermore, the mass ratio of the dispersant, the anti-settling agent and the charge repulsion agent is 10-1:1:10-1.

Furthermore, the mass ratio of the dispersant, the anti-settling agent and the charge repulsion agent is preferably 4-1:1:5-1.

Furthermore, the mass ratio of the dispersant, the anti-settling agent and the charge repulsion agent is most preferably 4:1:4.

The anti-settling agent, dispersant and charge repulsive agent of the present invention work synergistically, and utilize functional groups such as hydroxyl and carboxyl groups of the polymer in the anti-settling agent to form strong hydrogen bonding with amino groups and hydroxyl groups in the dispersant, thereby forming a thixotropic grid structure in the entire grinding liquid system, and coating the abrasives (aluminum oxide, silicon dioxide and zirconium oxide) in the formed space grid through adsorption and entanglement, so that the abrasives can maintain a completely dispersed and suspended state during long-term static standing; because the surface of the abrasive carries negative charge, it can adsorb the positive charge repulsive agent with amino groups to form a dense double electric layer coating structure, enhance the electrostatic repulsion between the abrasives, promote the full dispersion of the abrasives and the wear debris particles, and under the grinding shearing action, the hydrogen bonding action disappears, the abrasives and the wear debris particles still maintain a dispersed state, ensure that the abrasives can be quickly spread on the grinding disc surface, and are evenly dispersed and not easy to agglomerate, effectively increase the service life of the grinding liquid, and improve the grinding efficiency.

Furthermore, the wetting agent is one or more of fatty alcohol polyoxyethylene ether, fatty alcohol ethoxylate TERIC168, alkylphenol polyoxyethylene ether, nonylphenol polyoxyethylene ether and octylphenol polyoxyethylene ether.

Furthermore, the fatty alcohol polyoxyethylene ether is one or more of fatty alcohol polyoxyethylene ether AEO-9, fatty alcohol polyoxyethylene ether AEO-7 and fatty alcohol polyoxyethylene ether AEO-12.

Furthermore, the alkylphenol polyoxyethylene ether is alkylphenol polyoxyethylene ether TX-10 and/or alkylphenol polyoxyethylene ether TX-11.

Furthermore, the nonylphenol polyoxyethylene ether is one or more of nonylphenol polyoxyethylene ether NP-6, nonylphenol polyoxyethylene ether NP-7 and nonylphenol polyoxyethylene ether NP-9.

Furthermore, the octylphenol polyoxyethylene ether is one or more of octylphenol polyoxyethylene ether TRITONX-45, octylphenol polyoxyethylene ether TRITONX-100 and octylphenol polyoxyethylene ether TRITONX-15.

Furthermore, the wetting agent is preferably alkylphenol polyoxyethylene ether TX-10.

Furthermore, the wetting agent is 1-3 parts.

Furthermore, the defoaming agent is selected from one or more of dimethylsiloxane, ethylene glycol etherified polydimethylsiloxane, propylene glycol etherified polydimethylsiloxane and acetylene glycol polydimethylsiloxane.

Furthermore, the defoaming agent is preferably propylene glycol etherified polydimethylsiloxane.

Furthermore, the defoaming agent is 0.1-0.5 parts.

Furthermore, the ratio of the wetting agent to the defoaming agent is 1-20:1.

Furthermore, the ratio of the wetting agent to the defoaming agent is preferably 1-5:1.

Furthermore, the ratio of the wetting agent to the defoaming agent is more preferably 4:1.

The invention adopts a compounding scheme of a wetting agent and a defoaming agent with extremely low dynamic surface tension, effectively improves the dynamic wetting and penetration ability of the grinding liquid, ensures that the abrasive can be quickly spread on the grinding disk surface during the grinding process, and the grinding liquid can quickly penetrate into the micro cracks on the surface of the gallium arsenide sheet, thereby improving the grinding rate and grinding uniformity. At the same time, combined with the rapid defoaming and effective foam suppression capabilities of the defoaming agent, it is ensured that the grinding liquid will not generate foam during the stirring and grinding process, and the foam is prevented from reducing the effective contact area of the abrasive, resulting in reduced grinding efficiency; and the amphiphilic solvent can effectively and uniformly disperse the defoaming agent in the grinding liquid system, and the defoaming agent is added under the condition of high-speed shear stirring, and is quickly dispersed and emulsified into a microemulsion, so as to promote the defoaming agent to form a microemulsion and stably disperse, without demulsification and coagulation, thereby ensuring that the grinding liquid remains stable for a long time, and avoiding stratification and precipitation of the defoaming agent.

Furthermore, the amphiphilic solvent is a water-soluble solvent having a lipophilic group and a hydrophilic group.

Furthermore, the amphiphilic solvent is one or more of ethylene glycol monobutyl ether, propylene glycol butyl ether, triethylene glycol butyl ether, ethylene glycol hexyl ether, propylene glycol methyl ether, ethylene glycol tert-butyl ether, ethyl ethoxypropionate, diethylene glycol tert-butyl ether acetate and propylene glycol phenyl ether.

Furthermore, the amphiphilic solvent is preferably triethylene glycol butyl ether.

Furthermore, the amphiphilic solvent is 50-60 parts.

Another object of the present invention is to disclose a method for preparing a high-wetting, high-dispersion, high-suspending and easy-to-clean grinding aid, comprising the following steps:

Step (1): adding an amphiphilic solvent to a stirred tank, then adding a dispersant to completely dissolve the amphiphilic solvent, and then adding a wetting agent and a charge repulsive agent to make the wetting agent and the charge repulsive agent more easily dispersed, thereby obtaining a clear and transparent solution;

Step (2): adding a defoamer to the solution obtained in step (1) under stirring, starting high-speed dispersing stirring, and fully dispersing the defoamer through high shearing to form a soluble microemulsion that is evenly distributed in the system;

Step (3): adding an anti-settling agent to the solution obtained in step (2) under stirring, stirring and mixing evenly, and preparing a wetting, highly dispersed, highly suspended, and easily cleanable grinding aid.

Furthermore, the stirring time in step (1) is 10-20 min.

Furthermore, in step (2), a defoaming agent is added under stirring at 50-100 r/min.

Furthermore, the rotation speed of the high-speed dispersing stirring in step (2) is 500-2000 r/min.

Furthermore, the rotation speed of the high-speed dispersing stirring in step (2) is preferably 1000-2000 r/min.

Furthermore, the high-speed dispersing stirring time in step (2) is 10-30 minutes.

Furthermore, the high-speed dispersing stirring time in step (2) is preferably 10-20 min.

Furthermore, the stirring time in step (3) is 10-30 min.

Furthermore, the stirring time in step (3) is preferably 10-20 min.

Another object of the present invention is to disclose the use of a high-wetting, high-dispersing, high-suspending and easy-to-clean grinding aid in the field of hard and brittle material grinding liquid.

Furthermore, the hard and brittle material is gallium phosphide, gallium arsenide, indium phosphide or aluminum gallium arsenide.

Furthermore, the hard and brittle material is preferably gallium arsenide.

Another object of the present invention is to disclose a grinding liquid, comprising the above-mentioned high-wetting, high-dispersion, high-suspending, and easy-to-clean grinding aid and abrasive.

Furthermore, the amount ratio of the grinding aid to the abrasive is 8-1:1.

Furthermore, the ratio of the grinding aid to the abrasive is preferably 5-2:1.

Furthermore, the abrasive is one or more of silicon dioxide, aluminum oxide and zirconium oxide.

Furthermore, the abrasive is preferably silicon dioxide, aluminum oxide and zirconium oxide.

Furthermore, the abrasive comprises the following components in weight proportion:

Silicon dioxide 1-5 parts;

Alumina 10-30 parts;

Zirconium oxide 1-5 parts.

Furthermore, the silica particle size D50=0.5-10 μm.

Furthermore, the silica particle size is preferably D50=0.5-5 μm.

Furthermore, the silicon dioxide is 3-5 parts.

Furthermore, the aluminum oxide is selected from one or more of white corundum, brown corundum and semi-brittle corundum.

Furthermore, the aluminum oxide is preferably white corundum.

Furthermore, the particle size of the white corundum is D50=5-10 μm.

Furthermore, the particle size of the white corundum is preferably D50=8-10 μm.

Furthermore, the brown corundum particle size D50 is 5-20 μm.

Furthermore, the particle size of the brittle corundum is D50=5-20 μm.

Furthermore, the aluminum oxide is 10-20 parts.

Furthermore, the zirconium oxide particle size D50=5-10 μm.

Furthermore, the zirconium oxide particle size is preferably D50=5-8 μm.

Furthermore, the zirconium oxide is 1-3 parts.

The grinding liquid of the present invention comprises large-sized high-hardness aluminum oxide, zirconium oxide and small-sized low-hardness silicon dioxide composite abrasive with irregular morphology, and the small-sized silicon dioxide is coated on the surface of large-sized aluminum oxide and zirconium oxide to form a soft buffer layer on the surface of aluminum oxide and zirconium oxide. It is preferred to avoid direct hard contact between the edges of the large-sized high-hardness abrasive and the surface of gallium arsenide during the grinding process, so as to avoid deep scratches while ensuring the grinding efficiency. At the same time, the nano-sized silicon dioxide can undergo chemical mechanical polishing with the protruding part of the corrosion layer on the surface of the gallium arsenide to repair the corrosion pits and shallow scratches, and further reduce the surface roughness of the gallium arsenide after grinding.

Another object of the present invention is to disclose a method for preparing a grinding liquid, comprising the following steps: adding abrasive to a high-wetting, high-dispersing, high-suspending, and easy-to-clean grinding aid under stirring, stirring and mixing evenly, and obtaining a grinding liquid.

Further, abrasive is added under stirring at 50-100 r/min.

Furthermore, the stirring time is 10-60 min.

Furthermore, the stirring time is preferably 30-60 min.

Another object of the present invention is to disclose a use of a grinding liquid in the field of grinding hard and brittle materials.

Furthermore, the hard and brittle material is gallium phosphide, gallium arsenide, indium phosphide or aluminum gallium arsenide.

Furthermore, the hard and brittle material is preferably gallium arsenide.

Further, the gallium arsenide is ground with a grinding liquid, including the following grinding processes:

Pressure: 250kg, rotation speed: 30rpm, flow rate: 0.8L/min; disk temperature: 20-30℃; grinding time: 10min.

The high-wetting, high-dispersion, high-suspending, easy-to-clean grinding aid, preparation method, use and grinding liquid containing the same of the present invention have the following advantages compared with the prior art:

1) The anti-settling agent, dispersant and charge repulsion agent of the present invention work synergistically, and utilize the functional groups such as hydroxyl and carboxyl of the polymer in the anti-settling agent to form strong hydrogen bonding with the amino and hydroxyl groups in the dispersant, thereby forming a thixotropic grid structure in the entire grinding liquid system, and through the adsorption and entanglement effect, the abrasive (aluminum oxide, silicon dioxide and zirconium oxide) is coated in the formed space grid, so that it can maintain a completely dispersed and suspended state during a long period of static standing; because the surface of the abrasive carries a negative charge, it can adsorb the positive charge repulsion agent with amino groups to form a dense double electric layer coating structure, enhance the electrostatic repulsion between the abrasives, and promote the full dispersion of the abrasives and the wear debris particles. Under the grinding shearing action, the hydrogen bonding effect disappears, and the abrasives and the wear debris particles still remain in a dispersed state, ensuring that the abrasive can be quickly spread on the grinding disc surface, and is evenly dispersed and not easy to agglomerate, effectively increasing the service life of the grinding liquid and improving the grinding efficiency.

2) The present invention adopts a wetting agent and a defoaming agent compounding scheme with extremely low dynamic surface tension, which effectively improves the dynamic wetting and penetration ability of the grinding liquid, ensures that the abrasive can be quickly spread on the grinding disk surface during the grinding process, and the grinding liquid can quickly penetrate into the micro cracks on the surface of the gallium arsenide sheet, thereby improving the grinding rate and grinding uniformity. At the same time, combined with the rapid defoaming and effective foam suppression capabilities of the defoaming agent, it is ensured that the grinding liquid will not generate foam during the stirring and grinding process, thereby avoiding the foam from reducing the effective contact area of the abrasive and causing a decrease in grinding efficiency; and the amphiphilic solvent can effectively disperse the defoaming agent evenly in the grinding liquid system, add the defoaming agent under high-speed shear stirring conditions, quickly disperse and emulsify it into a microemulsion, promote the defoaming agent to form a microemulsion and stably disperse, without demulsification and coagulation, ensure that the grinding liquid remains stable for a long time, and avoid stratification and precipitation of the defoaming agent.

3) The grinding liquid of the present invention comprises irregularly shaped large-sized high-hardness aluminum oxide, zirconium oxide and small-sized low-hardness worm-like silicon dioxide composite abrasives, and the small-sized silicon dioxide is coated on the surface of the large-sized aluminum oxide and zirconium oxide to form a soft buffer layer on the surface of the aluminum oxide and zirconium oxide. It is preferred to avoid direct hard contact between the edges of the large-sized high-hardness abrasive and the surface of the gallium arsenide during the grinding process, thereby ensuring the grinding efficiency and avoiding the generation of deep scratches. At the same time, the nano-sized silicon dioxide can undergo chemical mechanical polishing with the protruding part of the corrosion layer on the surface of the gallium arsenide to repair the corrosion pits and shallow scratches, and further reduce the surface roughness of the gallium arsenide after grinding.

In summary, the grinding aid of the present invention has extremely high surface dynamic wetting and penetration ability, the contact angle can be as low as 25-30°, the surface tension is less than 30dyn/cm, and the composite defoaming technology is adopted so that the grinding liquid containing it produces almost no foam during stirring and grinding, and can quickly spread on the surface of gallium arsenide, and can quickly penetrate into the micro cracks on the surface of gallium arsenide to form a splitting effect, thereby improving the grinding efficiency; at the same time, the grinding aid has a good dispersing and anti-settling effect on mixed abrasives such as aluminum oxide, silicon dioxide, and zirconium oxide, which can avoid the agglomeration of different micropowders and grinding chips during the grinding process, and can make different types of abrasives evenly distributed in the grinding liquid and keep suspended for a long time. When the grinding liquid of the present invention is used for grinding, gallium arsenide is subjected to uniform force, the grinding rate is fast, the surface roughness after grinding is low, the TTV is low, the flatness is good and there are no obvious scratches, it is easy to clean, and there is no impurity residue on the surface. Therefore, the grinding aid and grinding liquid of the present invention have good application prospects and large-scale industrial promotion potential.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG1 is a diagram showing the dirty state of the surface of gallium arsenide ground in Comparative Example 1 after being rinsed with water, magnified 200 times under a microscope;

FIG2 shows the dirty state of the surface of gallium arsenide ground in Example 13 after being rinsed with water, magnified 200 times under a microscope;

FIG3 is a comparison photo of the suspension properties of the polishing liquid after being placed for 1 month, with the left side being Comparative Example 1 and the right side being Example 13;

FIG4 is a photograph of surface scratches of gallium arsenide after grinding in Comparative Example 1 observed under a microscope at a magnification of 200 times;

FIG5 is a photograph of the surface scratches of the gallium arsenide after grinding in Example 13 observed under a microscope at a magnification of 200 times.

DETAILED DESCRIPTION

The present invention is further described below in conjunction with embodiments:

Examples 1-12

Examples 1-12 disclose a variety of high-wetting, high-dispersion, high-suspending, and easy-to-clean grinding aids, the components and weight ratios of which are shown in Table 1, and the preparation methods thereof are as follows:

Step (1): add an amphiphilic solvent, a dispersant, a wetting agent and a charge repulsion agent into a stirring tank in sequence, stir for 20 minutes to mix evenly, and obtain a clear and transparent solution.

Step (2): add a defoamer to the solution obtained in step (1) under stirring at 50/min, start high-speed dispersion stirring to fully disperse the organosilicon defoamer to form a soluble microemulsion, and stir at 1000r/min for 30min to form a uniform and stable solution.

Step (3): add an anti-settling agent to the solution obtained in step (2) at 1000 r/min and stir for 30 min until the mixture is uniformly mixed.

Table 1 Components and contents of high wetting, high dispersibility, high suspension and easy-to-clean grinding aids of Examples 1-12

Characterization of the grinding aids described in Examples 1-12: After the grinding aids were diluted to 3%, the pH was 8-10, the conductivity was 500-1500 μs/cm, and the surface tension was 25-30 dyn/cm.

Examples 13-24

Examples 13-24 disclose a variety of polishing liquids, the components and weight ratios of which are shown in Table 2, and the preparation methods thereof are as follows:

Step (1): add an amphiphilic solvent, a dispersant, a wetting agent and a charge repulsion agent into a stirring tank in sequence, stir for 20 minutes to mix evenly, and obtain a clear and transparent solution.

Step (2): add a defoamer to the solution obtained in step (1) while stirring at 100 r/min, start high-speed dispersing stirring to fully disperse the organosilicon defoamer to form a soluble microemulsion, and stir at 1000 r/min for 30 minutes until a uniform and stable solution is formed.

Step (3): add an anti-settling agent to the solution obtained in step (2) at 1000 r/min and stir for 30 min until the mixture is uniformly mixed.

Step (4): adding alumina, zirconia and silica abrasives at 1000 r/min and stirring for 60 min to form a uniformly mixed suspension, thereby completing the preparation of the grinding liquid.

Table 2 Components and weight ratios of the grinding fluids of Examples 13-24

Comparative Examples 1-8

Comparative Examples 1-8 disclose a variety of grinding liquids, the components and weight ratios of which are shown in Table 3, and the preparation methods are the same as those of Example 13.

Table 3 Components and weight ratios of the grinding fluids of Comparative Examples 1-8

Performance Testing

Next, various properties of the above-mentioned polishing fluids were tested, as follows.

Figure 1 shows the surface dirtiness of gallium arsenide after being rinsed with water after being ground by comparative example 1, magnified 200 times under a microscope, and Figure 2 shows the surface dirtiness of gallium arsenide after being rinsed with water after being ground by example 13, magnified 200 times under a microscope. It can be seen that the surface of example 13 is clean without any particles or organic matter residue, while the surface of comparative example 1 has a small amount of residual particles and dirt (the place indicated by the arrow is dirt).

FIG3 is a comparison photo of the suspension properties of the grinding liquid after being placed for one month. The left side shows that the abrasive in Example 1 completely sinks to the bottom, while the right side shows that the abrasive in Example 13 still remains completely suspended.

Figure 4 is a photo of the surface scratches of the gallium arsenide after grinding in comparative example 1 observed under a microscope at a magnification of 200 times, and Figure 5 is a photo of the surface scratches of the gallium arsenide after grinding in example 13 observed under a microscope at a magnification of 200 times. It can be seen that comparative example 1 has obvious deep scratches, while example 13 has no deep scratches.

Table 4 shows the performance test data of Examples 13-24 and Comparative Examples 1-8. It can be seen that the polishing liquids of Examples 13-24 have high suspension, high dispersion and high wetting properties, fast removal rate, low scratches, low roughness and less surface dirt on the gallium arsenide surface after polishing.

Table 4 Performance test data of Examples 13-24 and Comparative Examples 1-8

in:

The test method is as follows:

The polishing liquids prepared in the above Examples 13-24 and Comparative Examples 1-8 were tested on a 4-inch GaAs wafer to compare the removal rate, TTV, TIR, Warp, Ra, maximum scratch width, damage layer depth, surface dirt, suspension, contact angle and surface tension.

Surface quality test after cleaning: first use the cleaning solution to perform two stages of ultrasonic cleaning at 50°C for 10 minutes, then use deionized water to perform ultrasonic cleaning at 50°C for 3 minutes, blow dry, and observe the surface quality under an optical microscope.

Maximum scratch width test after grinding: Use an optical microscope to test the maximum scratch width of the cleaned GaAs wafer under the same magnification and field of view, and measure it three times to get the average value.

Suspension test: Observe the suspension of the grinding liquid after standing for 1 month to see if it is stratified.

Contact angle and surface tension test: A contact angle meter was used to test the contact angle and surface tension of the polishing fluid on the gallium arsenide surface for 30 seconds.

Grinding process:

Grinding equipment: grinder;

GaAs size: 4 inches;

Speed: 30r/min;

Pressure: 100kg/plate;

Plate temperature: 30-40℃;

Grinding liquid flow rate: 0.9L/min;

Grinding time: 20min.

Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein by equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims (8)

1. The grinding aid is characterized by comprising the following components in parts by weight:

1-5 parts of dispersing agent;

0.1-5 parts of anti-settling agent;

1-5 parts of charge repulsive force agent;

1-5 parts of wetting agent;

0.1-1 part of defoaming agent;

40-60 parts of amphiphilic solvent;

the dispersing agent is one or more of maleic acid-acrylic acid copolymer, maleic acid-olefin copolymer and polyvinylpyrrolidone-vinylimidazole copolymer;

the anti-settling agent is one or more of hydroxyethyl cellulose, alkali-swelling polyurethane, alkali-soluble acrylic polymer and polyvinyl alcohol;

the charge repulsive agent is one or more of diethylenetriamine, triethylenetetramine, tetraethyl pentamine, DL-aminopropanediol, aminopentanol, N- (3-aminopropyl) diethanolamine, dicyclohexylamine, isopropanolamine and diglycolamine;

the wetting agent is one or more of fatty alcohol polyoxyethylene ether, fatty alcohol ethoxy compound TERIC168 and alkylphenol polyoxyethylene;

the amphiphilic solvent is one or more of ethylene glycol monobutyl ether, propylene glycol butyl ether, triethylene glycol butyl ether, ethylene glycol hexyl ether, propylene glycol methyl ether, ethylene glycol tertiary butyl ether, ethoxypropionic acid ethyl ester, diethylene glycol tertiary butyl ether acetate and propylene glycol phenyl ether.

2. The high wetting, high dispersing, high suspending and easy cleaning grinding aid according to claim 1, wherein the antifoaming agent is one or more selected from the group consisting of dimethyl siloxane, glycol etherified polydimethylsiloxane, propylene glycol etherified polydimethylsiloxane and acetylenic diol polydimethylsiloxane.

3. A process for preparing a highly wetting, highly dispersed, highly suspended, easily washable grinding aid according to any one of claims 1-2, comprising the steps of:

step (1): adding an amphiphilic solvent into a stirring kettle, then adding a dispersing agent to completely dissolve the amphiphilic solvent, and then adding a wetting agent and a charge repulsive force agent to prepare a clear and transparent solution;

step (2): adding an antifoaming agent into the solution obtained in the step (1) under stirring, and starting high-speed dispersion stirring to fully disperse the antifoaming agent to form a soluble microemulsion;

step (3): adding an anti-settling agent into the microemulsion obtained in the step (2) under stirring, and uniformly stirring and mixing to obtain the grinding aid with high wetting, high dispersion, high suspension and easy cleaning.

4. Use of a highly wetting, highly dispersing, highly suspending, easily cleanable grinding aid according to any one of claims 1 to 2 in the field of grinding fluids for hard and brittle materials.

5. A polishing slurry comprising the highly wetting, highly dispersed, highly suspended, easily cleanable polishing aid and abrasive according to any one of claims 1 to 2.

6. The polishing slurry of claim 5, wherein the abrasive is one or more of silica, alumina, and zirconia.

7. The grinding fluid of claim 5, wherein the abrasive comprises the following components in parts by weight:

1-5 parts of silicon dioxide;

10-30 parts of aluminum oxide;

1-5 parts of zirconia.

8. Use of a grinding fluid according to any one of claims 5-7 in the field of grinding of hard and brittle materials.