CN103013345B

CN103013345B - Oily diamond grinding liquid and preparation method thereof

Info

Publication number: CN103013345B
Application number: CN201210560797.1A
Authority: CN
Inventors: 潘国顺; 罗桂海; 罗海梅; 黄灿容
Original assignee: SHENZHEN LEAGUER MATERIAL CO Ltd; Tsinghua University; Shenzhen Research Institute Tsinghua University
Current assignee: SHENZHEN LEAGUER MATERIAL CO Ltd; Tsinghua University; Shenzhen Research Institute Tsinghua University
Priority date: 2012-12-21
Filing date: 2012-12-21
Publication date: 2015-02-18
Anticipated expiration: 2032-12-21
Also published as: CN103013345A

Abstract

The invention discloses an oily diamond grinding liquid and a preparation method thereof, and belongs to the technical field of surface superfine grinding. The grinding liquid comprises the following components by weight percent: 0.001%-10% of diamond micro powder, 0.001%-20% of surface active agent, 0-20% of dispersant, 0-10% of pH value regulator, 0-10% of wetting agent and oil in balancing amount. The oily diamond grinding liquid is mainly applied to surface grinding and polishing of silicon carbide wafers, LED sapphire substrate slices, ceramic, optical fiber, dies, semi-conductor compound wafers and the like. By the use of the oily diamond grinding liquid provided by the invention, the polishing efficiency can be greatly improved; the dispersing performance is good; a uniform and stable state can be kept for a long time; the degree of finish of products polished with the oily diamond grinding liquid is high; the polishing effect is good; no ingredient harmful to human body is contained; the cleaning is easy; and the environmental protection is facilitated.

Description

Oily diamond grinding fluid and preparation method thereof

Technical Field

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

Background

Diamond micropowder is an ultra-fine abrasive with high hardness and good mechanical and physical properties, is spherical or ellipsoidal in shape, and can not scratch a ground body when being used for grinding and polishing, so that the diamond micropowder is widely applied to different processing and polishing fields, particularly the ultra-precise surface polishing processing field at present. Diamond micropowder is an ideal polishing material for hard substances such as hard alloy, ceramics, gemstones, optical glass, artificial crystals, integrated circuits and the like, can be prepared into polishing products of paste, aerosol, membrane, oily or aqueous liquid, and limits the application range of diamond paste and aerosol due to the defects of easy settlement, difficult dispersion, large waste and the like. Compared with aqueous grinding fluid, the oily grinding fluid has the advantages of good lubricating property, high grinding speed, stable speed and cooling effect, and the aqueous grinding fluid is easy to cause large scratches on workpieces in the grinding process and has poor suspension stability, so the oily grinding fluid is relatively widely applied, but the traditional oily grinding fluid has the defects of easy precipitation, low polishing efficiency, corrosiveness, difficulty in cleaning, incapability of meeting the requirement of environmental protection and the like. The current research is mainly directed to the water-based diamond grinding fluid, and the research on the oil-based diamond grinding fluid is rarely reported.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provides an oily diamond grinding fluid and a preparation method thereof. The oil-based diamond grinding fluid provided by the invention is applied to grinding and polishing of ultra-precise surfaces, can greatly improve polishing efficiency, has good dispersion performance, can be stored for a long time without sedimentation, has high product smoothness after being polished by the oil-based diamond grinding fluid, has good polishing effect, does not contain components harmful to human bodies, does not corrode equipment, is easy to clean, and is beneficial to environmental protection.

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

The invention provides an oily diamond grinding fluid which is characterized by comprising diamond micro powder, a surfactant, a dispersant, a pH value regulator, a wetting agent and oil, wherein the weight percentage (wt.%) of each component is as follows:

diamond micro powder: 0.001% -10%;

surfactant (b): 0.001% -20%;

dispersing agent: 0% -20%;

pH value regulator: 0% -10%;

wetting agent: 0% -10%;

the balance being oil;

wherein the surfactant is one or more of nonionic surfactant, anionic surfactant or cationic surfactant, the nonionic surfactant is one or more of castor oil polyoxyethylene ether (preferably EL-n, n =10-90, HEL-20, HEL-40 and HEL-60), polyoxyethylene laurate, polyoxyethylene oleate, polyoxyethylene stearate, polyoxyethylene fatty amine, block polyoxyethylene-polyoxypropylene ether, fatty alcohol polyoxyethylene ether, polyoxyethylene alkylolamide, 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. The weight percentage of the surfactant is preferably 0.01 to 10%, more preferably 0.1 to 7%.

The dispersing agent is one or more of polyethylene glycol, ethylene glycol, polypropylene glycol, hexyldecanol, sodium hexametaphosphate, sodium tripolyphosphate, sodium pyrophosphate, sodium polyacrylate, polyacrylic acid, gum arabic powder, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose, carboxymethyl cellulose, hydroxypropyl methyl cellulose, N-methyl pyrrolidone, polyvinylpyrrolidone, sodium silicate and silane coupling agent. The dispersant is preferably present in an amount of 0.01 to 10% by weight, more preferably 0.01 to 1% by weight.

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

The grinding fluid can also comprise a pH value regulator, the pH value regulator is one or more 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 value regulating range of the grinding fluid is 3-11.

The grinding liquid can also comprise a wetting agent, wherein the wetting agent is one or more of glycerol, ethyl acetate, 1, 2-propylene glycol, 1, 3-propylene glycol, glycerol, 1, 3-butanediol, 1, 4-butanediol, lauryl alcohol, triethanolamine and cocamidopropyl betaine. The wetting agent is preferably present in an amount of 0.01 to 6% by weight, more preferably 0.5 to 2% by weight.

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.

The invention provides an oily diamond grinding fluid which comprises the following components in parts by weight:

the invention provides a preparation method of the oily diamond grinding fluid, which comprises the following specific steps:

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

2) Mixing the 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.

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

1) the diamond grinding fluid can realize good matching of mechanical action and chemical action, and has high polishing efficiency and good polishing quality. The diamond grinding fluid can be applied to thinning and grinding of LED sapphire substrate slices and silicon carbide wafers, and can also be used for grinding and polishing the surfaces of precision ceramics, precision molds, optical fibers, semiconductor compound wafers and the like.

2) The diamond grinding fluid has good dispersion performance, and can be stored for a long time to keep a uniform and stable state without sedimentation.

3) The diamond grinding fluid has high product smoothness and good polishing effect, does not contain components harmful to human bodies, is easy to clean and is beneficial to environmental protection.

Detailed Description

The invention is further illustrated by the following examples, which, of course, should not be construed as in any way limiting its scope.

(examples)

Taking specific example 1 as an example:

example 1: (1000 g of oily Diamond polishing solution prepared)

The grinding fluid in the embodiment comprises the following components in percentage by weight:

0.1 percent of 3 micron diamond polycrystalline micro powder

Surfactant lauric acid polyoxyethylene ester 1%

Surfactant sodium alpha-olefin sulfonate 1%

The balance is 3# industrial grade white oil, and the production area is as follows: the name is petrochemical.

10 g of polyoxyethylene laurate as a surfactant and 10 g of sodium alpha-olefin sulfonate as a surfactant were added to 979 g of white oil, and sufficiently stirred for 5 minutes.

And mixing 1 g of polycrystalline diamond micro powder with the granularity of 3 microns with the oily liquid, stirring and carrying out ultrasonic treatment for 15 minutes to fully wet the surface of the diamond micro powder, thus preparing the oily grinding fluid.

The method for preparing the oily diamond grinding fluid of the embodiments 2 to 6 comprises the following specific steps:

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

2) mixing diamond micropowder with the oily liquid, fully stirring and carrying out ultrasonic treatment for 15 minutes;

3) adding a dispersing agent into the oily liquid, fully stirring and ultrasonically dispersing for 15 minutes;

And (3) polishing process: the polishing machine is a single-side polishing machine, the polishing disk is a copper disk, the pressure is 5kgf, the rotating speed is 80rpm/min, the polishing time is 10min, and the flow rate of the polishing solution is 2 ml/min.

Polishing rate: the polishing removal rate is obtained by calculating the thickness change of the LED substrate slice before and after polishing, the average value is obtained by adopting a five-point method for measurement, the thickness change of the LED substrate slice before and after polishing can be measured by a micrometer, and the polishing rate is the ratio of the polishing removal thickness change to the polishing time.

Under the polishing process conditions, the grinding fluid is used for processing a 2-inch LED substrate slice, the surface roughness value (Ra) before polishing is 27.546nm, the surface roughness value (Ra) after polishing reaches 4.642nm, and the polishing rate reaches 1.25 microns/min.

The above description is only one embodiment of the present invention, and it should be noted that it is obvious to those skilled in the art that various modifications and improvements can be made without departing from the technical principle of the present invention, and these modifications and improvements should also be considered as the protection scope of the present invention.

The following table shows the components and contents of the oily diamond grinding fluid in each example, and the surface roughness and removal rate of the LED substrate sheet polished by the oily diamond grinding fluid.

Claims

1. The application method of the oily diamond grinding fluid is characterized in that the grinding fluid consists of diamond micro powder, a surfactant, a dispersing agent, a pH value regulator, a wetting agent and oil, and the weight percentage of each component is as follows:

diamond micro powder: 0.001% -10%;

surfactant (b): 0.001% -20%;

dispersing agent: 0.01% -10%;

pH value regulator: 0 to 10 percent;

wetting agent: 0.01% -6%;

the balance being oil;

the preparation method of the oily diamond grinding fluid comprises the following steps:

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 a pH value regulator into the dispersed oily liquid, fully stirring, and regulating the pH value to 3-11 to prepare oily grinding liquid;

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 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;

the dispersing agent is one or more of ethylene glycol, polypropylene glycol, hexyldecanol, sodium hexametaphosphate, sodium tripolyphosphate, sodium pyrophosphate, sodium polyacrylate, gum arabic powder, N-methyl pyrrolidone, polyvinylpyrrolidone and sodium silicate;

the pH value regulator is one or more of octadecylamine, isopropanolamine, 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 value regulating range of the grinding fluid is 3-11;

the wetting agent is one or more of ethyl acetate, lauryl alcohol, triethanolamine and cocamidopropyl betaine;

the oily diamond grinding fluid is used for thinning and grinding LED sapphire substrate slices and silicon carbide wafers, or is used for grinding and polishing the surfaces of precision ceramics, precision molds, optical fibers and semiconductor compound wafers.

2. The application method of claim 1, wherein the diamond micro powder is 0.05-2 wt%, the wetting agent is 0.5-2 wt%, the surfactant is 0.1-7 wt%, and the dispersant is 0.01-1 wt%.

3. The method of use according to claim 1, wherein the fine diamond powder is diamond single crystal or polycrystalline body, and the diamond crystal grain size is 1 to 9 μm.

4. The application method of claim 1, wherein the oil is one or more of mineral oil, synthetic oil and base oil.