CN105950115A - Environment-friendly abrasive paste suitable for gallium oxide substrate and preparation method of environment-friendly abrasive paste - Google Patents

Abstract

The invention discloses an environmentally friendly grinding paste suitable for gallium oxide substrates and a preparation method thereof. The grinding paste is composed of the following components in mass fractions: 0.5-10% of the main grinding agent, 0.5-10% of the grinding aid, Excipient 10‑50%, surfactant 0.5‑30%, thickener 0.3‑5%, complexing agent 0.3‑5%, preservative 0.1‑0.3%, defoamer 0.05‑0.3%, deionized water 30‑80%. Preparation method: stir deionized water and thickener, heat up after stirring, add excipient, complexing agent, grinding aid, stir, add surfactant, defoamer, stir homogeneously, form water phase; The grinding agent is pulverized to form a solid phase; the water phase and the solid phase are stirred and homogenized, and then the preservative is added, and the stirring is continued until the homogeneity is obtained. The abrasive paste prepared by the invention is friendly to the environment and operators, and at the same time can alleviate the cleavage phenomenon on the gallium oxide surface.

Description

A kind of environment-friendly grinding paste suitable for gallium oxide substrate and preparation method thereof

technical field

The invention belongs to the technical field of grinding paste, and in particular relates to an environmentally friendly grinding paste suitable for gallium oxide substrates and a preparation method thereof.

Background technique

In January 2013, at the "Japan 3rd LED and Organic EL Lighting Exhibition" held in Tokyo, Tamura Manufacturing Co., Ltd. and its subsidiary Lightwave Corporation exhibited the gallium oxide single crystal (β-Ga ₂ O ₃ ) white LEDs, compared with the traditional use of ordinary blue LED chips made on sapphire substrates, has the characteristics of easily increasing the light output power, so it has attracted widespread attention in the industry. Because gallium oxide single crystal materials are new crystal materials, the current related technologies such as crystal growth and ultra-precision processing technology are not mature, so there are not many reports on the production technology related to gallium oxide substrates. Even in Japan, only the oxidation The finished products of gallium substrates and the LED devices made of them rarely involve the preparation process technology of gallium oxide substrates.

Abrasive paste is one of the most common auxiliary consumables in the process of crystal material processing, but the abrasive paste is not universal. Because different crystal materials have different physical and chemical properties, such as soft and brittle lithium niobate and lithium tantalate, high-hard and brittle silicon carbide and sapphire, deliquescent potassium dihydrogen phosphate, brittle and easy-to-cleavage gallium oxide, etc. Uncomfortable phenomena may occur when processing the above-mentioned crystals with a general-purpose abrasive paste, so it is necessary to develop a more scientific and reasonable special-purpose polishing paste. In addition, some abrasive pastes on the market or in earlier patents contain less used or avoided chemicals that are often harmful to humans or the environment, such as nonylphenol ethoxylates and octylphenol Polyoxyethylene ether surfactants.

Contents of the invention

In order to overcome the deficiencies of the prior art above, the present invention provides an environmentally friendly abrasive paste suitable for gallium oxide substrates and a preparation method thereof, which is friendly to the environment and operators, and can alleviate the cleavage phenomenon on the surface of gallium oxide.

The technical scheme adopted in the present invention is:

An environmentally friendly grinding paste suitable for gallium oxide substrates, consisting of the following components in mass fractions: main grinding agent 0.5-10%, grinding aid 0.5-10%, excipient 10-50%, surfactant 0.5-30%, thickener 0.3-5%, complexing agent 0.3-5%, preservative 0.1-0.3%, defoamer 0.05-0.3%, deionized water 30-80%.

Preferably, the above-mentioned main grinding agent is a mixture of one or more of corundum, silicon carbide, and synthetic diamond, with a particle size of 0.25-5 μm.

Preferably, the above-mentioned grinding aid is a mixture of one or more of sodium hydroxide, potassium hydroxide, dimethylamine, triethanolamine, dimethylethylamine, diethylenetriamine, cyclohexylamine, and di-n-butylamine .

Preferably, the above-mentioned excipients are one or a mixture of sorbitol, glycerol, polyethylene glycol, polypropylene glycol, polyglycerol 10, and fatty acid monoglycerides.

Preferably, the above-mentioned surfactant is alkanolamide, fatty amide sulfosuccinic acid monoester, sodium N-lauroyl sarcosinate, fatty alcohol polyoxyethylene ether sodium sulfate, sodium lauryl sulfate, potassium lauryl sulfate, woody Sulfonate, fatty alcohol polyoxyethylene ether or a mixture of several.

Preferably, the above thickener is one of carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose, carrageenan, xanthan gum, hydroxypropyl guar gum, carbomer, polyacrylic acid species or a mixture of several species.

Preferably, the complexing agent is one or a mixture of disodium edetate, tetrasodium edetate, sodium gluconate, and sodium citrate.

Preferably, the above-mentioned preservative is Kethon preservative.

Preferably, the above-mentioned defoamer is one of polyether defoamers and silicone defoamers.

A method for preparing an environmentally friendly abrasive paste suitable for gallium oxide substrates, comprising the following steps:

(1) Add deionized water and thickener to the agitator, stir to dissolve and heat up to 60-80°C, add excipients, complexing agents, grinding aids in turn, stir to dissolve, then add surfactants, Defoamer, stirring, homogenizing, forming an aqueous phase;

(2) Put the main grinding agent in the powder tank and pulverize to form a solid phase;

(3) Add water phase and solid phase to the vacuum paste making machine, stir for homogenization, add preservative, continue stirring for homogeneity, and obtain the environmentally friendly abrasive paste suitable for gallium oxide substrates.

The functions of each component are as follows:

Main grinding agent: the hardness is higher than that of gallium oxide. Under the action of pressure, the surface and subsurface damage layer of the crystal plane of gallium oxide substrate caused by the previous processing process is removed by shearing.

Grinding aid: It has the effect of corroding the surface of gallium oxide crystal, making gallium oxide form a softer basic compound, restraining the occurrence of cleavage fracture of the processed crystal plane, and helping the main grinding agent to grind gallium oxide crystal faster.

Surfactants, complexing agents and thickeners: adsorbed on the surface of abrasive particles, balance and neutralize the surface free energy of abrasive particles, so that the main abrasive particles will no longer bond and agglomerate during the production process of the abrasive paste, It has the effect of uniformly dispersing the abrasive in the grinding paste and preventing aggregation; during the grinding process, it is adsorbed on the surface of the ground gallium oxide fine waste, and disperses and wraps it, in the joint of the grinding disc (or grinding pad) and the water flow Under the action, the processing waste is taken out of the grinding interface; in the process of preparing the grinding paste and grinding the substrate substrate, the adhesion and fluidity of the grinding paste are improved, which is more conducive to the preparation, production and grinding application of the grinding paste; neutralize the grinding The charge generated by the friction between the grinding disc (or grinding pad) and the surface of the substrate during the process can eliminate the adhesion of pollutants in the processed environment on the surface of the workpiece and improve the quality of the grinding crystal surface.

Excipients are used to improve the moisture retention of the grinding paste, and play the role of plasticizing, lubricating, dispersing and suspending during the application process, and can be used for coloring the grinding paste with different specifications and uses, which is convenient for classified use.

Preservatives: prevent the chemical components in the grinding paste from being corrupted and deteriorated due to chemical changes and other reasons.

Defoaming agent: eliminate the foam generated during the grinding process due to the application of surfactants, and prevent the foam from interfering with the smooth progress of the grinding process.

The grinding paste prepared by the present invention has the following advantages:

(1) Environmentally friendly components are used without adding surfactants such as nonylphenol ethoxylates and octylphenol ethoxylates, which are friendly to the environment and operators;

(2) It is suitable for gallium oxide substrates, can alleviate the cleavage phenomenon on the surface of gallium oxide, and fills the gap in the prior art.

Description of drawings

Fig. 1 is the surface topography figure of wafer before grinding of embodiment 5;

Fig. 2 is the surface topography figure of wafer after grinding of embodiment 5;

Fig. 3 is the surface topography figure of wafer before grinding of embodiment 6;

Fig. 4 is the wafer surface topography figure after grinding of embodiment 6;

Fig. 5 is the surface topography figure of wafer before grinding of embodiment 7;

Fig. 6 is a topography diagram of the wafer surface after grinding in Example 7.

detailed description

The present invention will be further described in detail through specific embodiments below.

Example 1

An environmentally friendly abrasive paste suitable for gallium oxide substrates, consisting of the following components in mass fractions: 0.5% silicon carbide (particle size: 0.5 μm), 0.5% cyclohexylamine, 17.75% glycerol, lignin sulfonate 0.5% salt, 0.3% hydroxyethyl cellulose, 0.3% sodium citrate, 0.1% Kaisong preservative, 0.05% silicone diethanol defoamer, 80% deionized water.

The preparation method comprises the following steps:

(1) Add deionized water and hydroxyethyl cellulose to the stirrer, stir at 60r/min for 10 minutes, heat up to 60°C after dissolving, add glycerol, sodium citrate, cyclohexylamine in sequence, and stir at 150r/min Stir at a speed of 1/min to dissolve, then add lignosulfonate and silicone diethanol antifoaming agent in sequence, stir at a speed of 150r/min for 20 minutes, and homogenize at a speed of 1500r/min for 10 minutes to form a water phase;

(2) Put the silicon carbide in the powder tank and pulverize it to form a solid phase;

(3) Add water phase and solid phase to the vacuum paste making machine, stir at 300r/min for 20 minutes at 30°C, then homogenize at 1500r/min for 10 minutes, add Kaisong preservative, 1500r/min Homogenize for 10 minutes, and then stir at 15 r/min for 20 minutes to obtain the environmentally friendly abrasive paste suitable for gallium oxide substrates.

Using the abrasive paste prepared in this embodiment, the gallium oxide substrate was ground on a precision grinding machine, the surface roughness of the wafer was reduced from 65 nm to 7 nm, and the surface cleavage phenomenon was significantly alleviated.

Example 2

An environmentally friendly abrasive paste suitable for gallium oxide substrates, consisting of the following components in mass fractions: 10% corundum (with a particle size of 5 μm), 10% dimethylamine, 10% polypropylene glycol, and N-lauroyl sarcosine Sodium Acetate 29.4%, Xanthan Gum 2%, Carbomer 3%, Sodium Gluconate 5%, Kaison Preservative 0.3%, Silicone Diethanol Antifoaming Agent 0.3%, Deionized Water 30%.

The preparation method comprises the following steps:

(1) Add deionized water, xanthan gum, and carbomer to the mixer, stir at 240r/min for 30 minutes, heat up to 80°C after dissolving, add polypropylene glycol, sodium gluconate, and dimethylamine in sequence, to Stir at 300r/min to dissolve, then add N-lauroyl sarcosinate and silicone diethanol defoamer in turn, stir at 300r/min for 40 minutes, and homogenize at 15000r/min for 30 minutes to form a water phase;

(2) Pulverize the corundum in a powder tank to form a solid phase;

(3) Add water phase and solid phase to the vacuum paste making machine, Stir at a rate of r/min for 40 minutes, then homogenize at a rate of 15000r/min for 30 minutes; Environmentally friendly abrasive paste for gallium oxide substrates.

Using the abrasive paste prepared in this embodiment, the gallium oxide substrate was ground on a precision grinding machine, the surface roughness of the wafer was reduced from 345nm to 189nm, and the surface cleavage phenomenon was significantly alleviated.

Example 3

An environmentally friendly abrasive paste suitable for gallium oxide substrates, consisting of the following components in mass fractions: silicon carbide 0.5% (particle size 5 μm), corundum 0.5% (particle size 5 μm), diethylenetriamine 2% , Fatty acid monoglyceride 50%, Potassium lauryl sulfate 10%, Hydroxypropyl guar gum 3%, Sodium gluconate 1%, Sodium citrate 1%, Tetrasodium edetate 1%, Kayson preservative 0.2%, simethicone 0.1%, deionized water 30.7%.

The preparation method comprises the following steps:

(1) Add deionized water, hydroxypropyl guar gum, sodium gluconate, and sodium citrate to the mixer, stir at 80r/min for 12 minutes, heat up to 60-80°C after dissolving, and add fatty acid monoglyceride in turn Esters, tetrasodium ethylenediaminetetraacetic acid, diethylenetriamine, stirring and dissolving at 180r/min, then adding potassium lauryl sulfate, simethicone, stirring at 180r/min for 25 minutes, at 2500r/min Homogenize for 15 minutes to form an aqueous phase;

(2) Put silicon carbide and corundum in a powder tank to pulverize to form a solid phase;

(3) Add water phase and solid phase to the vacuum paste making machine, Stir at a rate of r/min for 25 minutes, then homogenize at a rate of 2500r/min for 15 minutes; Environmentally friendly abrasive paste for gallium oxide substrates.

Using the abrasive paste prepared in this embodiment, the gallium oxide substrate was ground on a precision grinding machine, the surface roughness of the wafer was reduced from 339 nm to 177 nm, and the surface cleavage phenomenon was significantly alleviated.

Example 4

An environmentally friendly abrasive paste suitable for gallium oxide substrates, consisting of the following components in mass fractions: 5% silicon carbide (particle size 3 μm), 3% dimethylethylamine, 20% fatty acid monoglyceride, fat Amide sulfosuccinic acid monoester 30%, carrageenan 2%, tetrasodium edetate 2%, Kethon preservative 0.2%, simethicone 0.2%, deionized water 37.6%.

The preparation method comprises the following steps:

(1) Add deionized water and carrageenan to the mixer, stir at 220r/min for 25 minutes, heat up to 65°C after dissolving, add fatty acid monoglyceride, tetrasodium ethylenediaminetetraacetate, dimethyl ethyl alcohol in sequence Amine, stirred at 250r/min to dissolve, then added fatty amide sulfosuccinic acid monoester and simethicone in sequence, stirred at 280r/min for 35 minutes, and homogenized at 13000r/min for 25 minutes to form a water phase;

(2) Put the silicon carbide in the powder tank and pulverize it to form a solid phase;

(3) Add water phase and solid phase to the vacuum paste making machine, stir at 550r/min for 35 minutes at 55°C, then homogenize at 13000r/min for 25 minutes, add Kaisong preservative, 13000r/min Homogenize for 25 minutes, and then stir at 120 r/min for 50 minutes to obtain the environmentally friendly abrasive paste suitable for gallium oxide substrates.

Using the abrasive paste prepared in this embodiment, the gallium oxide substrate was ground on a precision grinding machine, the surface roughness of the wafer was reduced from 305nm to 167nm, and the surface cleavage phenomenon was significantly alleviated.

Example 5

An environmentally friendly abrasive paste suitable for gallium oxide substrates, consisting of the following components in mass fractions: W3 diamond powder 5.0% (particle size 1.5-3μm), potassium hydroxide 1.5%, di-n-butylamine 1.5%, Fatty acid monoglycerides 20%, polyethylene glycol 200 5%, Macrogol 1000 10%, Alkanolamide 1.5%, Fatty Amide Sulfosuccinic Acid Monoester 1.5%, Disodium EDTA 1.8%, Carbomer 2.0%, Kayson Preservative 0.2% , GP type glycerol polyether 0.1%, deionized water 49.9%.

The preparation method comprises the following steps:

(1) Add deionized water and carbomer to the mixer, stir at 110r/min for 18 minutes, heat up to 75°C after dissolving, add fatty acid monoglycerides, polyethylene glycol 200, polyethylene glycol 1000 in sequence , disodium edetate, potassium hydroxide, di-n-butylamine, stirred and dissolved at a rate of 200r/min, and then added alkanolamide, fatty amide sulfosuccinic acid monoester, GP glycerol polyether, at 200r/min Stir at a speed of 10000r/min for 30 minutes, and homogenize for 20 minutes at a speed of 10000r/min to form an aqueous phase;

(2) Put the diamond powder in the powder tank and pulverize it to form a solid phase;

(3) Add water phase and solid phase to the vacuum paste making machine, stir at 450r/min for 30 minutes at 45°C, then homogenize at 10,000r/min for 20 minutes, add Kaisong preservative, 10,000r/min Homogenize for 20 minutes, and then stir for 40 minutes at a rate of 100 r/min to obtain the environmentally friendly abrasive paste suitable for gallium oxide substrates.

Using the abrasive paste prepared in this example, grind the gallium oxide substrate substrate on a precision grinder, and use the Keyence three-dimensional morphology instrument to observe the crystal surface morphology. The surface morphology of the wafer before grinding is shown in Figure 1. After grinding The surface morphology of the wafer is shown in Figure 2. The surface roughness of the wafer is reduced from 296nm to 155nm, and the surface cleavage phenomenon is obviously alleviated.

Example 6

An environmentally friendly abrasive paste suitable for gallium oxide substrates, consisting of the following components in mass fractions: W1.5 diamond micropowder 5.0% (particle size 0.75-1.5μm), sodium hydroxide 1.0%, triethanolamine 1.0% , Glycerin 15.0%, Sorbitol 30.0%, Sodium Fatty Alcohol Polyoxyethylene Ether Sulfate 0.5%, Fatty Alcohol Polyoxyethylene Ether 0.5%, Disodium EDTA 1.3%, Hydroxypropyl Methyl Cellulose 0.5%, polyacrylic acid 0.5%, Kaisong preservative 0.2%, GP type glycerol polyether 0.1%, deionized water 43.9%.

The preparation method comprises the following steps:

(1) Add deionized water and polyacrylic acid to the mixer, stir at 150r/min for 20 minutes, heat up to 70°C after dissolving, add glycerol, sorbitol, disodium edetate, hydrogen Sodium oxide and triethanolamine were stirred and dissolved at a rate of 200r/min, and then fatty alcohol polyoxyethylene ether sodium sulfate, fatty alcohol polyoxyethylene ether, and GP glycerol polyether were added successively, stirred at a rate of 250r/min for 30 minutes, and then stirred at a rate of 9000r/min. /min rate of homogenization for 15 minutes to form an aqueous phase;

(2) Put the diamond powder in the powder tank and pulverize it to form a solid phase;

(3) Add water phase and solid phase to the vacuum paste making machine, Stir at a rate of r/min for 35 minutes, then homogenize at a rate of 9000r/min for 20 minutes; Environmentally friendly abrasive paste for gallium oxide substrates.

Using the abrasive paste prepared in this example, grind the gallium oxide substrate substrate on a precision grinder, and use the Keyence three-dimensional morphology instrument to observe the crystal surface morphology. The surface morphology of the wafer before grinding is shown in Figure 3. After grinding The surface morphology of the wafer is shown in Figure 4, the surface roughness of the wafer is reduced from 185nm to 35nm, and the surface cleavage phenomenon is obviously alleviated.

Example 7

An environmentally friendly abrasive paste suitable for gallium oxide substrates, consisting of the following components in mass fractions: W0.5 diamond powder 5.0% (particle size 0.25-0.5μm), sodium hydroxide 1.5%, triethanolamine 1.5% , Polyglycerin 10 35%, Sodium Lauryl Sulfate 1.5%, Fatty Alcohol Polyoxyethylene Ether 0.5%, Sodium Gluconate 1.0%, Carboxymethyl Cellulose 1.8%, Kayson Preservative 0.2%, GPE Polyoxyethylene Polyethylene Oxypropylene glyceryl ether 0.1%, deionized water 43.9%.

The preparation method comprises the following steps:

(1) Add deionized water and carboxymethyl cellulose to the mixer, stir at 200r/min for 20 minutes, heat up to 70°C after dissolving, add polyglycerol 10, sodium gluconate, sodium hydroxide, triethanolamine in sequence , stir and dissolve at a rate of 200r/min, then add sodium lauryl sulfate, fatty alcohol polyoxyethylene ether, GPE polyoxyethylene polyoxypropylene glyceryl ether in sequence, stir at a rate of 200r/min for 30 minutes, and mix at a rate of 8000r/min Matter for 20 minutes to form an aqueous phase;

(2) Put the diamond powder in the powder tank and pulverize it to form a solid phase;

(3) Add water phase and solid phase to the vacuum paste making machine, Stir at a rate of r/min for 30 minutes, then homogenize at a rate of 8000r/min for 20 minutes, add Kaisong preservative, homogenize at a rate of 8000r/min for 20 minutes, and stir at a rate of 80r/min for 40 minutes to obtain the said Environmentally friendly abrasive paste for gallium oxide substrates.

Using the abrasive paste prepared in this example, grind the gallium oxide substrate substrate on a precision grinder, and use the Keyence three-dimensional morphology instrument to observe the crystal surface morphology. The surface morphology of the wafer before grinding is shown in Figure 5, and after grinding The surface morphology of the wafer is shown in Figure 6, the surface roughness of the wafer is reduced from 62nm to 5nm, and the surface cleavage phenomenon is obviously alleviated.

Claims (10)

1. An environmentally friendly grinding paste suitable for gallium oxide substrates, characterized in that it consists of the following components in mass fractions: main grinding agent 0.5-10%, grinding aid 0.5-10%, excipient 10- 50%, surfactant 0.5-30%, thickener 0.3-5%, complexing agent 0.3-5%, preservative 0.1-0.3%, defoamer 0.05-0.3%, deionized water 30-80%. 2. A kind of environment-friendly grinding paste suitable for gallium oxide substrates according to claim 1, characterized in that: the main grinding agent is a mixture of one or more of corundum, silicon carbide, and synthetic diamond, and the particle size is 0.25-5μm. 3. A kind of environment-friendly grinding paste suitable for gallium oxide substrate according to claim 1, characterized in that: said grinding aid is sodium hydroxide, potassium hydroxide, dimethylamine, triethanolamine, dimethyl One or more mixtures of ethylamine, diethylenetriamine, cyclohexylamine, and di-n-butylamine. 4. A kind of environment-friendly grinding paste suitable for gallium oxide substrate according to claim 1, characterized in that: said excipient is sorbitol, glycerol, polyethylene glycol, polypropylene glycol, polyglycerol 10. One or more mixtures of fatty acid monoglycerides. 5. A kind of environment-friendly grinding paste suitable for gallium oxide substrates according to claim 1, characterized in that: the surfactant is alkanolamide, fatty amide sulfosuccinic acid monoester, N-lauroyl succinic acid One or more mixtures of sodium phosphate, sodium fatty alcohol polyoxyethylene ether sulfate, sodium lauryl sulfate, potassium lauryl sulfate, lignin sulfonate, and fatty alcohol polyoxyethylene ether. 6. A kind of environment-friendly grinding paste suitable for gallium oxide substrate according to claim 1, characterized in that: the thickener is carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose One or more mixtures of gluten, carrageenan, xanthan gum, hydroxypropyl guar gum, carbomer, and acrylic polymer. 7. A kind of environment-friendly grinding paste suitable for gallium oxide substrates according to claim 1, characterized in that: the complexing agent is disodium edetate, tetrasodium edetate, gluconic acid One or more mixtures of sodium and sodium citrate. 8. An environmentally friendly abrasive paste suitable for gallium oxide substrates according to claim 1, characterized in that: the preservative is Kaisong preservative. 9. An environmentally friendly abrasive paste suitable for gallium oxide substrates according to claim 1, wherein the defoamer is one of polyether defoamers and silicone defoamers. 10. The preparation method of a kind of environment-friendly grinding paste suitable for gallium oxide substrates according to claim 1, characterized in that: comprising the following steps: (1) Add deionized water and thickener to the agitator, stir to dissolve and heat up to 60-80°C, add excipients, complexing agents, grinding aids in turn, stir to dissolve, then add surfactants, Defoamer, stirring, homogenizing, forming an aqueous phase; (2) Put the main grinding agent in the powder tank and pulverize to form a solid phase; (3) Add water phase and solid phase to the vacuum paste making machine, stir for homogenization, add preservative, continue stirring for homogeneity, and obtain the environmentally friendly abrasive paste suitable for gallium oxide substrates.