CN103013345B - Oily diamond grinding liquid and preparation method thereof - Google Patents

Oily diamond grinding liquid and preparation method thereof Download PDF

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Publication number
CN103013345B
CN103013345B CN201210560797.1A CN201210560797A CN103013345B CN 103013345 B CN103013345 B CN 103013345B CN 201210560797 A CN201210560797 A CN 201210560797A CN 103013345 B CN103013345 B CN 103013345B
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acid
sodium
oil
polishing
polyoxyethylene
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Expired - Fee Related
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CN103013345A (en
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潘国顺
罗桂海
罗海梅
黄灿容
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SHENZHEN LEAGUER MATERIAL CO Ltd
Tsinghua University
Shenzhen Research Institute Tsinghua University
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SHENZHEN LEAGUER MATERIAL CO Ltd
Tsinghua University
Shenzhen Research Institute Tsinghua University
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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

Oiliness diamond grinding fluid and preparation method thereof
Technical field
The present invention relates to a kind of for grinding, the polishing fluid, particularly a kind of oiliness diamond grinding fluid and preparation method thereof of polishing, belong to superfinish grinding and polishing technical field.
Background technology
Diadust is a kind of ultra-fine abrasive material with high rigidity and good mechanical physicals, its profile is spherical or elliposoidal, polished body can not be scratched for grinding and polishing, therefore be widely used in different processing polished fields, particularly ultra-precision surface polishing field at present.Diadust is the desirable polishing material of one of the hard material such as Wimet, pottery, jewel, opticglass, artificial lens, unicircuit, the polished product of paste, aerosol, membranaceous, oiliness or waterborne liquid can be made, diamond paste, aerosol disperse due to precipitation of easily stammering, difficulty and waste the shortcomings such as larger, limit its range of application.Oiliness lapping liquid is compared with aqueous polishing liquid, oiliness lapping liquid lubricity is good, grinding speed is fast, rate stabilization also has cooling down effect, and aqueous polishing liquid easily causes workpiece to occur large cut in process of lapping, suspension stability is poor, therefore, the application of oiliness lapping liquid is relatively extensive, but traditional oiliness lapping liquid easily precipitates, polishing efficiency is low, have corrodibility and non-easy cleaning, do not meet the shortcomings such as the requirement of environmental protection.Current research is mainly for water diamond lapping liquid, and the research also rarely seen report to oiliness diamond grinding fluid.
Summary of the invention
The object of the invention is the weak point in order to overcome prior art, proposing a kind of oiliness diamond grinding fluid and preparation method thereof.Oiliness diamond grinding fluid provided by the invention is applied to the grinding and polishing of superfinish, polishing efficiency can be improved greatly, dispersing property is good, long-term storage can there is not sedimentation, high by product glossiness after its polishing, polishing effect is good and not containing harmful composition, not etching apparatus, be easy to cleaning, be conducive to environmental protection.
In order to realize above-mentioned target, present invention utilizes tensio-active agent and modification is carried out to particle, make diamond particles can keep good dispersion state in oil, there is good stability and not easily scratch polishing sample again.Add the synergistic function with some additives, improve the polishing speed of oiliness diamond grinding fluid and obtain good polishing effect.
Oiliness diamond grinding fluid provided by the invention, is characterized in that, this lapping liquid is made up of diadust, tensio-active agent, dispersion agent, pH value regulator, wetting agent and oil, and the weight percentage (wt.%) of each composition is:
Diadust: 0.001%-10%;
Tensio-active agent: 0.001%-20%;
Dispersion agent: 0%-20%;
PH value regulator: 0%-10%;
Wetting agent: 0%-10%;
All the other are oil;
Wherein, described tensio-active agent is nonionogenic tenside, one or more in anion surfactant or cats product, described nonionogenic tenside is castor oil polyoxyethylene ether (preferred EL-n, n=10-90 and HEL-20, HEL-40, HEL-60), lauric acid polyoxyethylene ester, polyoxyethylene oleic acid ester, polyoxyethylene stearic acid ester, aliphatic amine polyoxyethylene ether, Block polyoxyethylene-polyethenoxy ether, fatty alcohol-polyoxyethylene ether, alkylol amide polyethylene oxide ether, alkyl glycoside, coconut oil fatty acid monoethanolamide, cocoanut fatty acid diethanolamide, ethylene glycol monostearate, Triglycol distearate, Zerol, Polyglycerine monostearate, sucrose fatty ester, sorbitan fatty acid ester, one or more in polyoxyethylene sorbitan fatty acid ester, described anion surfactant is one or more in C12-16 sodium alkyl benzene sulfonate, sulfonated alkyl naphathalene, C12-16 alkyl sodium sulfonate, alpha-olefin sodium sulfonate, sulfonated lignin, sulfonated petro-leum, C12-16 alkyl-sulphate, ricinolic acid butyl ester sodium sulfate, fatty alcohol polyoxyethylene ether sulfate, lauramide sodium ethyl sulfate, oleoyl amino acid sodium, N-acyl amino hydrochlorate, aliphatic alcohol polyethenoxy ether carboxylate, described cats product is one or more in tetrahydroglyoxaline, Dodecyl trimethyl ammonium chloride, Trimethyllaurylammonium bromide, 4 bromide, trimethyl ammonium sulfate.The preferred 0.01-10% of weight percentage of tensio-active agent, more preferably 0.1-7%.
Described dispersion agent is one or more in polyoxyethylene glycol, ethylene glycol, polypropylene glycol, hexyl decyl alcohol, Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, trisodium phosphate, sodium polyacrylate, polyacrylic acid, gum arabic powder, hydroxypropylcellulose, Vltra tears, Natvosol, carboxymethyl cellulose, HYDROXY PROPYL METHYLCELLULOSE, methylcellulose gum, N-Methyl pyrrolidone, polyvinylpyrrolidone, sodium silicate, silane coupling agent.The preferred 0.01-10% of weight percentage of dispersion agent, more preferably 0.01-1%.
Described diadust is diamond single crystal body or polycrystal, and diamond crystal particle diameter is 1-9 micron.The preferred 0.01-5% of weight percentage of diadust, more preferably 0.05-2%.
PH value regulator can also be comprised in lapping liquid, described pH value regulator is one or more in potassium hydroxide, sodium hydroxide, ammoniacal liquor, thanomin, trolamine, stearylamine, α-amino isopropyl alcohol, hydrochloric acid, sulfuric acid, nitric acid, boric acid, acetic acid, stearic acid, phenylformic acid, Sodium Benzoate, oleic acid, sodium oleate, Whitfield's ointment, lauric acid, vinylformic acid, tartrate, gallic acid, and the pH value regulation range of lapping liquid is 3-11.
Wetting agent can also be comprised in lapping liquid, described wetting agent is glycerine, ethyl acetate, 1,2-PD, 1,3-PD, glycerol, 1, one or more in 3-butyleneglycol, BDO, lauryl alcohol, trolamine, AMONYL 380LC.The preferred 0.01-6% of weight percentage of wetting agent, more preferably 0.5-2%.
Described oil is one or more in white oil, petroleum naphtha, mineral oil, synthetic oil, base oil, rapeseed oil, Viscotrol C, sweet oil, whiteruss.
A kind of oiliness diamond grinding fluid that the present invention proposes, its component and proportioning are:
The invention provides a kind of preparation method of above-mentioned oiliness diamond grinding fluid, concrete steps are:
1) wetting agent, tensio-active agent and oil are mixed in proportion, fully stir 5-30 minute.
2) diadust is mixed with above-mentioned oily liquid, fully stir and ultrasonic 5-30 minute.
3) in above-mentioned oily liquid, add dispersion agent, fully stir and ultrasonic disperse 5-30 minute.
4) in above-mentioned scattered oily liquid, add pH value regulator, fully stir, adjust ph is 3-11, is namely prepared into oiliness lapping liquid.
The present invention compared with prior art has the following advantages:
1) diamond grinding fluid of the present invention can realize mechanical effect and the good matching of chemical action, and make polishing efficiency high, quality of finish is good.Diamond grinding fluid of the present invention can be applicable to the thinning grinding of LED Sapphire Substrate sheet and silicon carbide wafer, also may be used for the grinding and polishing on the surfaces such as high technology ceramics, precision compression molds, optical fiber and semiconductor compound wafer.
2) diamond grinding fluid dispersing property of the present invention is good, can long-term storage keep uniform and stable state sedimentation not to occur.
3) high by product glossiness after its polishing, polishing effect is good, and diamond grinding fluid of the present invention, not containing harmful composition, is easy to cleaning, is conducive to environmental protection.
Embodiment
Below by embodiment, the invention will be further elaborated, certainly in no case should be construed as limiting the scope of the invention.
(embodiment)
For specific embodiment 1:
Embodiment 1:(prepares the oiliness diamond grinding fluid of 1000 grams)
In the present embodiment each component of lapping liquid and weight percent as follows:
3 micron diamond polycrystalline powders 0.1%
Tensio-active agent lauric acid polyoxyethylene ester 1%
Tensio-active agent alpha-olefin sodium sulfonate 1%
All the other are 3# industrial grade white oil, the place of production: Maoming Petrochemical.
Get 10 grams of tensio-active agent lauric acid polyoxyethylene ester and 10 grams of tensio-active agent alpha-olefin sodium sulfonates add in the white oil of 979 grams, fully stir 5 minutes.
Getting 1 gram particle degree is that the polycrystalline diamond micro mist of 3 microns mixes with above-mentioned oily liquid, stirs and ultrasonic 15 minutes, and fully wetting diadust surface, is namely prepared into oiliness lapping liquid.
The preparation method of the oiliness diamond grinding fluid of embodiment 2-6, concrete steps are:
1) wetting agent, tensio-active agent and oil are mixed in proportion, fully stir 5 minutes;
2) diadust is mixed with above-mentioned oily liquid, fully stir and ultrasonic 15 minutes;
3) in above-mentioned oily liquid, add dispersion agent, fully stir and ultrasonic disperse 15 minutes;
4) in above-mentioned scattered oily liquid, add pH value regulator, fully stir, adjust ph is 3-11, is namely prepared into oiliness lapping liquid.
Glossing: polishing machine used is single side polishing machine, use polishing disk is copper dish, and pressure is 5kgf, and rotating speed is 80rpm/min, and polishing time is 10min, and polishing fluid flow is 2ml/min.
Polishing speed: polish removal rate is obtained by the change calculations of LED substrate slice thickness before and after polishing, five-spot measurement is adopted to average, before and after the polishing of test LED substrate slice, the available milscale of change of thickness records, and polishing speed is the ratio that variation in thickness and polishing time are removed in polishing.
Under above-mentioned polishing technological conditions, this lapping liquid is used to process the LED substrate slice of 2 cun, polishing front surface roughness value (Ra) is 27.546nm, and surface of polished roughness value (Ra) reaches 4.642nm, and polishing speed reaches 1.25 [mu.
The above is only wherein a kind of embodiment of the present invention; it should be noted that the those skilled in the art for the art; under the prerequisite not departing from the technology of the present invention principle; can also make corresponding adjustment and improve, these adjustment and improvement also should be considered as protection scope of the present invention.
Following table is component and the content of the medium oil diamond grinding fluid of each embodiment and is carried out the LED substrate slice surfaceness after polishing by it, removed speed.

Claims (4)

1. an application method for oiliness diamond grinding fluid, is characterized in that, this lapping liquid is made up of diadust, tensio-active agent, dispersion agent, pH value regulator, wetting agent and oil, and the weight percentage of each composition is:
Diadust: 0.001%-10%;
Tensio-active agent: 0.001%-20%;
Dispersion agent: 0.01%-10%;
PH value regulator: 0-10%;
Wetting agent: 0.01%-6%;
All the other are oil;
The preparation method of described oiliness diamond grinding fluid is as follows:
1) wetting agent, tensio-active agent and oil are mixed in proportion, fully stir 5-30 minute;
2) diadust is mixed with above-mentioned oily liquid, fully stir and ultrasonic 5-30 minute;
3) in above-mentioned oily liquid, add dispersion agent, fully stir and ultrasonic disperse 5-30 minute;
4) in above-mentioned scattered oily liquid, add pH value regulator, fully stir, adjust ph is 3-11, is namely prepared into oiliness lapping liquid;
Wherein,
Described tensio-active agent is nonionogenic tenside, one or more in anion surfactant or cats product, described nonionogenic tenside is castor oil polyoxyethylene ether, lauric acid polyoxyethylene ester, polyoxyethylene oleic acid ester, polyoxyethylene stearic acid ester, aliphatic amine polyoxyethylene ether, Block polyoxyethylene-polyethenoxy ether, fatty alcohol-polyoxyethylene ether, alkylol amide polyethylene oxide ether, alkyl glycoside, coconut oil fatty acid monoethanolamide, cocoanut fatty acid diethanolamide, ethylene glycol monostearate, Triglycol distearate, Zerol, Polyglycerine monostearate, sucrose fatty ester, one or more in polyoxyethylene sorbitan fatty acid ester, described anion surfactant is one or more in C12-16 sodium alkyl benzene sulfonate, sulfonated alkyl naphathalene, C12-16 alkyl sodium sulfonate, alpha-olefin sodium sulfonate, sulfonated lignin, sulfonated petro-leum, C12-16 alkyl-sulphate, ricinolic acid butyl ester sodium sulfate, fatty alcohol polyoxyethylene ether sulfate, lauramide sodium ethyl sulfate, oleoyl amino acid sodium, N-acyl amino hydrochlorate, aliphatic alcohol polyethenoxy ether carboxylate, described cats product is one or more in tetrahydroglyoxaline, Dodecyl trimethyl ammonium chloride, Trimethyllaurylammonium bromide, 4 bromide, trimethyl ammonium sulfate,
Described dispersion agent is one or more in ethylene glycol, polypropylene glycol, hexyl decyl alcohol, Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, trisodium phosphate, sodium polyacrylate, gum arabic powder, N-Methyl pyrrolidone, polyvinylpyrrolidone, sodium silicate;
Described pH value regulator is one or more in stearylamine, α-amino isopropyl alcohol, boric acid, acetic acid, stearic acid, phenylformic acid, Sodium Benzoate, oleic acid, sodium oleate, Whitfield's ointment, lauric acid, vinylformic acid, tartrate, gallic acid, and the pH value regulation range of lapping liquid is 3-11;
Described wetting agent is one or more in ethyl acetate, lauryl alcohol, trolamine, AMONYL 380LC;
Described oiliness diamond grinding fluid is used for the thinning grinding of LED Sapphire Substrate sheet and silicon carbide wafer, or for the grinding and polishing of high technology ceramics, precision compression molds, optical fiber and semiconductor compound wafer surface.
2. application method according to claim 1, it is characterized in that, the weight percentage of diadust is 0.05-2%, and the weight percentage of wetting agent is 0.5-2%, the weight percentage of tensio-active agent is 0.1-7%, and the weight percentage of dispersion agent is 0.01-1%.
3. application method according to claim 1, is characterized in that, diadust is diamond single crystal body or polycrystal, and diamond crystal particle diameter is 1-9 micron.
4. application method according to claim 1, is characterized in that, described oil is one or more in mineral oil, synthetic oil, base oil.
CN201210560797.1A 2012-12-21 2012-12-21 Oily diamond grinding liquid and preparation method thereof Expired - Fee Related CN103013345B (en)

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