CN103013345A - Oily diamond grinding liquid and preparation method thereof - Google Patents

Abstract

The invention discloses an oil-based diamond grinding liquid and a preparation method thereof, which belong to the technical field of surface superfine grinding. The grinding liquid contains the following components: diamond micropowder, surfactant, dispersant, pH regulator, wetting agent and Oil, the weight ratio (wt.) of each component is: diamond powder: 0.001%-10%; surfactant: 0.001%-20%; dispersant: 0-20%; pH regulator: 0-10 %; wetting agent: 0-10%; the rest is oil. It is mainly used in the grinding and polishing of silicon carbide wafers, LED sapphire substrates, ceramics, optical fibers, molds and semiconductor compound wafers. Using the abrasive liquid provided by the invention can greatly improve the polishing efficiency, has good dispersion performance, and can maintain a uniform and stable state for a long time. After polishing, the product has a high finish, good polishing effect and does not contain harmful ingredients to the human body. It is easy to clean and is conducive to environmental protection. .

Description

Oily diamond grinding liquid and preparation method thereof

technical field

The invention relates to a polishing liquid used for grinding and polishing, in particular to an oily diamond grinding liquid and a preparation method thereof, belonging to the technical field of ultra-fine surface grinding and polishing.

Background technique

Diamond micropowder is an ultra-fine abrasive with high hardness and good mechanical and physical properties. Its shape is spherical or ellipsoidal. It is used for grinding and polishing without scratching the object to be ground. Therefore, it has been widely used in different processing and polishing fields. Especially in the field of ultra-precision surface polishing. Diamond powder is an ideal polishing material for hard alloys, ceramics, gemstones, optical glass, artificial crystals, integrated circuits, etc. It can be made into ointment, aerosol, film, oily or water-based liquid polishing products, diamond Ointments and aerosols have limited their application scope due to their disadvantages such as easy stagnation and precipitation, difficulty in dispersing and large waste. Compared with water-based grinding fluid, oil-based grinding fluid has good lubricating performance, fast grinding speed, stable speed and cooling effect, while water-based grinding fluid is easy to cause large scratches on the workpiece during the grinding process, and the suspension stability is relatively low. Poor, therefore, the application of oil-based abrasives is relatively wide, but the traditional oil-based abrasives are prone to precipitation, low polishing efficiency, corrosive and difficult to clean, and do not meet the requirements of environmental protection. The current research is mainly aimed at water-based diamond grinding fluid, but the research on oil-based diamond grinding fluid is rarely reported.

Contents of the invention

The objective of the invention is to propose a kind of oily diamond grinding liquid and preparation method thereof in order to overcome the weak point of prior art. The oily diamond abrasive liquid provided by the invention is applied to the grinding and polishing of ultra-fine surfaces, which can greatly improve the polishing efficiency, has good dispersion performance, and can be stored for a long time without sedimentation. Harmful ingredients to the human body, no corrosion to equipment, easy to clean, and conducive to environmental protection.

In order to achieve the above goals, the present invention utilizes a surfactant to modify the particles, so that the diamond particles can maintain a good dispersion state in the oil, have good stability and are not easy to scratch the polished sample. Together with the synergistic effect of some additives, the polishing rate of the oily diamond grinding fluid is improved and a good polishing effect is obtained.

The oily diamond grinding liquid provided by the present invention is characterized in that the grinding liquid is composed of diamond micropowder, surfactant, dispersant, pH regulator, wetting agent and oil, and the weight percentage of each component (wt.% )for:

Diamond powder: 0.001%-10%;

Surfactant: 0.001%-20%;

Dispersant: 0%-20%;

pH regulator: 0%-10%;

Wetting agent: 0%-10%;

The rest is oil;

Wherein, the surfactant is one or more of nonionic surfactants, anionic surfactants or cationic surfactants, and the nonionic surfactants are castor oil polyoxyethylene ethers (preferably EL -n, n=10-90 and HEL-20, HEL-40, HEL-60), polyoxyethylene laurate, polyoxyethylene oleate, polyoxyethylene stearate, fatty amine polyoxyethylene ether , block polyoxyethylene-polyoxypropylene ether, fatty alcohol polyoxyethylene ether, alkyl alcohol amide polyoxyethylene ether, alkyl glycoside, coconut oil fatty acid monoethanolamide, coconut oil fatty acid diethanolamide, ethylene glycol Monostearate, polyethylene glycol distearate, glycerol monostearate, polyglycerol monostearate, sucrose fatty acid ester, sorbitan fatty acid ester, polyoxyethylene sorbitan One or more of alcohol fatty acid esters; the anionic surfactant is C12-16 sodium alkylbenzene sulfonate, alkyl naphthalene sulfonate, C12-16 sodium alkyl sulfonate, α-olefin sulfonate Sodium sulfonate, lignosulfonate, petroleum sulfonate, C12-16 alkyl sulfate, sodium butyl ricinoleate sulfate, fatty alcohol polyoxyethylene ether sulfate, sodium lauramide ethyl sulfate, oleoyl amino acid One or more of sodium, N-acyl amino acid salt, fatty alcohol polyoxyethylene ether carboxylate; the cationic surfactant is imidazoline, dodecyltrimethylammonium chloride, dodecane One or more of trimethylammonium bromide, tetramethylammonium bromide, and dodecyltrimethylammonium sulfate. The weight percentage of surfactant is preferably 0.01-10%, more preferably 0.1-7%.

The dispersant is polyethylene glycol, ethylene glycol, polypropylene glycol, hexyldecanol, sodium hexametaphosphate, sodium tripolyphosphate, sodium pyrophosphate, sodium polyacrylate, polyacrylic acid, gum arabic powder, hydroxypropyl Hydroxyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose, carboxymethyl cellulose, hydroxypropyl methyl cellulose, methyl cellulose, N-methylpyrrolidone, polyvinylpyrrolidone, natron , One or more of the silane coupling agents. The weight percentage of the dispersant is preferably 0.01-10%, more preferably 0.01-1%.

The diamond micropowder is diamond single crystal or polycrystal, and the diamond crystal grain size is 1-9 microns. The weight percentage of diamond micropowder is preferably 0.01-5%, more preferably 0.05-2%.

Can also include pH regulator in the grinding liquid, described pH regulator is potassium hydroxide, sodium hydroxide, ammoniacal liquor, ethanolamine, triethanolamine, octadecylamine, isopropanolamine, hydrochloric acid, sulfuric acid, nitric acid, boric acid , acetic acid, stearic acid, benzoic acid, sodium benzoate, oleic acid, sodium oleate, salicylic acid, lauric acid, acrylic acid, tartaric acid, gallic acid or one or more of them, and the pH value adjustment range of the grinding liquid is 3 -11.

Can also comprise wetting agent in the polishing liquid, described wetting agent is glycerin, ethyl acetate, 1,2-propanediol, 1,3-propanediol, glycerol, 1,3-butanediol, 1,4 - One or more of butylene glycol, lauryl alcohol, triethanolamine, and cocamidopropyl betaine. The weight percentage of the wetting agent is preferably 0.01-6%, more preferably 0.5-2%.

The oil is one or more of white oil, naphtha, mineral oil, synthetic oil, base oil, rapeseed oil, castor oil, olive oil, and liquid paraffin.

A kind of oily diamond abrasive liquid that the present invention proposes, its component and proportioning are:

The present invention provides a kind of preparation method of above-mentioned oily diamond grinding liquid, concrete steps are:

1) Mix the wetting agent, surfactant and oil in proportion and stir thoroughly for 5-30 minutes.

2) Mix the diamond micropowder with the above oily liquid, stir well and ultrasonic for 5-30 minutes.

3) Add dispersant to the above oily liquid, stir thoroughly and ultrasonically disperse for 5-30 minutes.

4) Add a pH adjuster to the dispersed oily liquid, stir well, and adjust the pH to 3-11 to prepare an oily grinding liquid.

Compared with the prior art, the present invention has the following advantages:

1) The diamond abrasive liquid of the present invention can achieve good matching between mechanical action and chemical action, so that the polishing efficiency is high and the polishing quality is good. The diamond grinding liquid of the present invention can be applied to thinning and grinding of LED sapphire substrates and silicon carbide wafers, and can also be used for grinding and polishing surfaces of precision ceramics, precision molds, optical fibers and semiconductor compound wafers.

2) The diamond abrasive liquid of the present invention has good dispersibility, and can be stored for a long time to maintain a uniform and stable state without sedimentation.

3) After polishing, the product has high finish and good polishing effect. The diamond grinding liquid of the present invention does not contain harmful components to the human body, is easy to clean, and is beneficial to environmental protection.

Detailed ways

The present invention will be further described below by way of examples, which certainly should not be construed as limiting the scope of the present invention in any case.

(Example)

Take specific embodiment 1 as an example:

Embodiment 1: (preparation of 1000 grams of oily diamond grinding fluid)

Each component of grinding liquid and its weight percent are as follows in the present embodiment:

3 micron diamond polycrystalline powder 0.1%

Surfactant polyoxyethylene laurate 1%

Surfactant Sodium α-Olefin Sulfonate 1%

The rest is 3# industrial grade white oil, origin: Maoming Petrochemical.

Get 10 grams of surfactant polyoxyethylene laurate and 10 grams of surfactant sodium α-olefin sulfonate and add them to 979 grams of white oil, and stir thoroughly for 5 minutes.

Take 1 gram of polycrystalline diamond powder with a particle size of 3 microns and mix it with the above-mentioned oily liquid, stir and sonicate for 15 minutes, fully wet the surface of the diamond powder, and prepare an oily grinding liquid.

The preparation method of the oily diamond grinding liquid of embodiment 2-6, concrete steps are:

1) Mix the wetting agent, surfactant and oil in proportion and stir thoroughly for 5 minutes;

2) Mix the diamond micropowder with the above oily liquid, stir thoroughly and ultrasonically for 15 minutes;

3) Add dispersant to the above oily liquid, stir thoroughly and ultrasonically disperse for 15 minutes;

4) Add a pH adjuster to the dispersed oily liquid, stir well, and adjust the pH to 3-11 to prepare an oily grinding liquid.

Polishing process: The polishing machine used is a single-sided polishing machine, the polishing disc is a copper disc, the pressure is 5kgf, the rotation speed is 80rpm/min, the polishing time is 10min, and the flow rate of the polishing solution is 2ml/min.

Polishing rate: The polishing removal rate is calculated by the change of the thickness of the LED substrate before and after polishing. The average value is measured by the five-point method. The thickness change of the test LED substrate before and after polishing can be measured with a micrometer. ratio of time.

Under the above polishing process conditions, use this abrasive to process a 2-inch LED substrate, the surface roughness (Ra) before polishing is 27.546nm, the surface roughness (Ra) after polishing reaches 4.642nm, and the polishing rate reaches 1.25 microns /minute.

The above is only one of the embodiments of the present invention. It should be pointed out that those skilled in the art can make corresponding adjustments and improvements without departing from the technical principle of the present invention. These adjustments and improvements should also be regarded as the protection scope of the present invention.

The following table shows the components and contents of the oily diamond grinding liquid in each embodiment, as well as the surface roughness and removal rate of the LED substrate after being polished by it.

Claims (9)

1. The oil-based diamond grinding fluid is characterized by comprising diamond micro powder, a surfactant, a dispersing agent, a pH value regulator, a wetting agent and oil, wherein the weight percentage of each component is as follows:

diamond micro powder: 0.001% -10%;

surfactant (b): 0.001% -20%;

dispersing agent: 0 to 20 percent;

pH value regulator: 0 to 10 percent;

wetting agent: 0 to 10 percent;

the balance being oil;

wherein,

the surfactant is one or more of a nonionic surfactant, an anionic surfactant or a cationic surfactant, and the nonionic surfactant is one or more of castor oil polyoxyethylene ether, polyoxyethylene laurate, polyoxyethylene oleate, polyoxyethylene stearate, fatty amine polyoxyethylene ether, block polyoxyethylene-polyoxypropylene ether, fatty alcohol polyoxyethylene ether, alkylolamide polyoxyethylene ether, alkyl glycoside, coconut oil fatty acid monoethanolamide, coconut oil fatty acid diethanolamide, ethylene glycol monostearate, polyethylene glycol distearate, glycerol monostearate, polyglycerol monostearate, sucrose fatty acid ester, sorbitan fatty acid ester and polyoxyethylene sorbitan fatty acid ester; the anionic surfactant is one or more of C12-16 sodium alkyl benzene sulfonate, alkyl naphthalene sulfonate, C12-16 sodium alkyl sulfonate, alpha-olefin sodium sulfonate, lignosulfonate, petroleum sulfonate, C12-16 alkyl sulfate, ricinoleic acid butyl ester sodium sulfate, fatty alcohol-polyoxyethylene ether sulfate, lauroyl aminoethyl sodium sulfate, oleamido sodium, N-acyl amino acid salt and fatty alcohol-polyoxyethylene ether carboxylate; the cationic surfactant is one or more of imidazoline, dodecyl trimethyl ammonium chloride, dodecyl trimethyl ammonium bromide, tetramethyl ammonium bromide and dodecyl trimethyl ammonium sulfate.

2. The polishing slurry according to claim 1, wherein the dispersant is one or more selected from the group consisting of polyethylene glycol, ethylene glycol, polypropylene glycol, hexyldecanol, sodium hexametaphosphate, sodium tripolyphosphate, sodium pyrophosphate, sodium polyacrylate, polyacrylic acid, gum arabic powder, hydroxypropyl cellulose, hydroxypropyl methylcellulose, hydroxyethyl cellulose, carboxymethyl cellulose, hydroxypropyl methylcellulose, methyl cellulose, N-methyl pyrrolidone, polyvinyl pyrrolidone, sodium silicate, and silane coupling agents.

3. The grinding fluid of claim 1, wherein the diamond micro powder is 0.01 to 5 wt%, the wetting agent is 0.01 to 6 wt%, the surfactant is 0.01 to 10 wt%, and the dispersant is 0.01 to 10 wt%.

4. The grinding fluid of claim 1, wherein the diamond micro powder is 0.05 to 2 wt%, the wetting agent is 0.5 to 2 wt%, the surfactant is 0.1 to 7 wt%, and the dispersant is 0.01 to 1 wt%.

5. The abrasive liquid according to claim 1, wherein the fine diamond powder is diamond single crystal or polycrystalline body, and the diamond crystal particle size is 1 to 9 μm.

6. The polishing slurry according to claim 1, wherein the pH regulator is one or more selected from the group consisting of potassium hydroxide, sodium hydroxide, ammonia water, ethanolamine, triethanolamine, octadecylamine, isopropanolamine, hydrochloric acid, sulfuric acid, nitric acid, boric acid, acetic acid, stearic acid, benzoic acid, sodium benzoate, oleic acid, sodium oleate, salicylic acid, lauric acid, acrylic acid, tartaric acid and gallic acid, and the pH of the polishing slurry is adjusted to be in a range of 3-11.

7. The grinding fluid of claim 1, wherein the wetting agent is one or more of glycerol, ethyl acetate, 1, 2-propanediol, 1, 3-propanediol, glycerol, 1, 3-butanediol, 1, 4-butanediol, lauryl alcohol, triethanolamine, and cocamidopropyl betaine.

8. The polishing slurry according to claim 1, wherein the oil is one or more selected from white oil, naphtha, mineral oil, synthetic oil, base oil, rapeseed oil, castor oil, olive oil, and liquid paraffin.

9. The method for producing an oil-based diamond polishing liquid according to any one of claims 1 to 8, characterized by comprising the steps of:

1) mixing the wetting agent, the surfactant and the oil in proportion, and fully stirring for 5-30 minutes;

2) mixing diamond micropowder with the oily liquid, stirring thoroughly, and performing ultrasonic treatment for 5-30 min;

3) adding a dispersing agent into the oily liquid, fully stirring and ultrasonically dispersing for 5-30 minutes;

4) adding pH regulator into the dispersed oily liquid, stirring, and regulating pH to 3-11 to obtain oily grinding liquid.