CN102433190B - Diamond linear cutting fluid and preparation method thereof - Google Patents
Diamond linear cutting fluid and preparation method thereof Download PDFInfo
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- CN102433190B CN102433190B CN 201110325955 CN201110325955A CN102433190B CN 102433190 B CN102433190 B CN 102433190B CN 201110325955 CN201110325955 CN 201110325955 CN 201110325955 A CN201110325955 A CN 201110325955A CN 102433190 B CN102433190 B CN 102433190B
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- cutting liquid
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Abstract
The invention discloses diamond linear cutting fluid and a preparation method thereof. By adding a polyphenol compound into propylene glycol(PG) cutting fluid, the action of radicals generated by pyrolysis of a small amount of PG in a linear cutting process can be eliminated, chain reaction of radicals can be prevented, and thus, the complete components of PG can be stabilized. The diamond linear cutting fluid is reasonably designed and can be used simply with convenient operation, the use effect of the diamond linear cutting fluid is good, and the practical value of the diamond linear cutting fluid is high, and the drawbacks of serious pollution and high chip pollution rate of the conventional silicon chip cutting fluid are overcome.
Description
Technical field
The present invention relates to a kind of silicon chip cutting auxiliary material technical field, particularly relate to a kind of diamond wire cutting liquid and preparation method thereof.
Background technology
Silicon chip is the base mateiral of industries such as semi-conductor, sun power and liquid-crystal display, be divided into monocrystalline silicon piece and polysilicon chip, its raw material is silicon single crystal or polysilicon, pulls into silicon ingot through ingot furnace, be cut into silicon rod again, use wire cutting machine to be processed into the silicon chip of all size afterwards.
Propylene glycol (writing a Chinese character in simplified form PG) has excellent lubrication and cooling performance, can be used as the diamond wire cutting liquid, accounts for about 65%～75% (all the other compositions mainly are water) of cutting liquid proportional.The wetting property of PG and space steric effect mainly rely on the poly-hydroxy group in its molecular structure to realize, and hydroxyl quantity is more many in the PG molecule, building block is more long, and its wetting property and space steric effect will be more strong.PG cutting liquid is to be the product of principal constituent with PG, this series products has nontoxic, non-stimulated, has good water-solubility, and have with many organic constituentses good characteristics such as consistency are arranged, this product has the buoyancy of uphanging, high lubricity and high dispersive characteristic, to cut liquid and be attached to equably on the cutting wire, thereby and move next the realization fast by steel wire the dicing of silicon chip is processed.
PG has excellent lubrication and cooling property because of its frictional coefficient little (about 0.28), the big characteristics such as (about 3J/gK) of specific heat to electroplating the diamond line of cut, thereby plays important effect in diamond line cutting silicon chip process.PG is stable under normal operation, but when temperature rises to 300 ℃ of left and right sides, fracture takes place and degrades in building block, generate formaldehyde, acetaldehyde and propenal etc., wherein formaldehyde and acetaldehyde are gaseous state and toxic to human body at normal temperatures, and propenal is the cacodorous liquid of water white transparency under normal conditions.And multi-line cutting machine can produce a large amount of grinding heats in the process of cutting silicon rod, learns according to correlative study, and the thermograde that forms on the grinding top layer can reach 600～1000 ℃.In our actual test, learn, the about 300L of the PG cutting each usage quantity of liquid, but last recovery can only obtain about 270L, and the 10%PG that namely has an appointment cutting liquid at high temperature is cracked into other volatile component, thereby influences cutting effect.
The reaction of the Pintsch process of PG is to produce free radical by the homogeneous phase cracking, produces also by the polymer molecule that causes other from free radical chain reactions that scission reaction realizes again.Its reaction process is as follows:
Can find out that from above-mentioned reaction process PG at high temperature mainly is cracked into the material of non-hydroxyls such as formaldehyde, acetaldehyde and propenal, its oilness and cooling property will be greatly affected, thereby influence diamond line cutting silicon chip quality.And because the loss of PG will need to replenish new cutting liquid at every turn, thereby increase diamond line cutting silicon chip cost.
In the silicon chip of the diamond line cutting at present process, usually use the water-soluble cutting liquid as the main body composition with PG, after cutting liquid is applied to the multi-thread cutting of silicon chip, the waste slurry that cutting produces will be recycled usually, be that waste slurry gets PG cutting liquid and contains silica flour and the solid slag two portions of a small amount of diamond through solid-liquid separation, wherein about 90% (namely each about 10% being depleted) of the PG cutting liquid rate of recovery need be replenished about 10% new PG cutting liquid and be mixed with cutting liquid when reusing.
By reclaiming the repeated use of cutting liquid, can effectively reduce the silicon chip production cost, realize that useless cutting liquid turns waste into wealth, reduce environmental pollution and realize the recycling of resource.
But there is certain limitation in the prior art:
1, cutting liquid is after using, and variation has taken place for himself performance, causes oilness and cooling performance to descend as PG through Pintsch process.These must impact the cutting result, and the yield rate that causes cutting silicon chip is lower.
2, PG itself is nontoxic, but after high temperature uses, the part material is arranged at normal temperatures for gaseous state (as formaldehyde etc.) and harmful in the cracking composition, be passed to the cutting machine outside easily, and silicon chip process zone relative closure, so operator and peripheral staff there is disadvantageous effect.
Summary of the invention
The present invention be directed to the deficiencies in the prior art, a kind of diamond wire cutting liquid of the stable propylene glycol cutting liquid moiety that a kind of input cost is low, interpolation is convenient and result of use is good, practical value is high and preparation method thereof is provided.
On the one hand, the invention provides a kind of diamond wire cutting liquid, contain propylene glycol cutting liquid, also contain polyphenolic compound.
PG that the present invention mentions cutting liquid is business-like cutting liquid on the market.
The polyphenolic compound that the present invention mentions refers to have in the molecular structure general name of the chemical substance of several phenolic hydroxyl groups, comprises polyphenols such as pycnogenols class, flavonoid, tannins, phenolic acids and anthocyanin class, but is not limited thereto.Preferably, described polyphenolic compound is selected from one or more in pycnogenols class, flavonoid, tannins, phenolic acids and the anthocyanin class.
Preferably, described polyphenolic compound is Powdered.
Preferably, the weight percent of polyphenolic compound in the diamond wire cutting liquid is 0.1%～5.0% in the step (1).
The invention also discloses a kind of preparation method of diamond wire cutting liquid simultaneously, may further comprise the steps:
(1) each component weighing: polyphenolic compound and propylene glycol cutting liquid are carried out weighing respectively;
(2) preparation diamond wire cutting liquid: get institute's weighing in the step (1) polyphenolic compound, be added in the propylene glycol cutting liquid, fully stir dissolving down, make the diamond wire cutting liquid.
Propylene glycol that the present invention mentions cutting liquid is business-like cutting liquid on the market.
Preferably, the weight percent of polyphenolic compound in propylene glycol cutting liquid is 0.1%～5.0% in the step (1).
Preferably, when fully stirring in the step (2), churning time is 0.5～1 hour.
Polyphenolic compound is fabulous hydrogen proton or electron donor, and it can form stable phenols free radical intermediate, makes superoxide or other free radical become stable hydroperoxide, thereby stops the generation of chain reaction, and namely chain stops provides agent.And himself is because resonance delocalization and be not fit to the position of molecular oxygen attack, can not cause new free radical or because chain reaction and by oxidation rapidly is more stable.The high reaction activity that replaces owing to its hydroxyl and have the ability of engulfing free radical and show good Green Tea Extract ability.
Polyphenolic compound stops the mechanism of free chain reaction to be: the phenolic hydroxyl group on the free radical attack phenolic compound forms a middle transition attitude, and the transfer of transfer transport and hydrogen proton takes place then, the final phenolic hydroxyl group free radical that forms the energy stable existence.The phenolic hydroxyl group free radical is because the stability that the resonance effect produces makes it than other free radical torpescence more, be difficult for and other organic molecule generation free chain reaction, so can play the effect of eliminating free radical, and phenolic hydroxyl group group number is more many in the polyphenolic compound, provide hydrogen proton ability more strong, the ability of removing free radical is more high.
Pycnogenols, English name are Oligomeric Proantho Cyanidins (OPC), are a kind of Vitamin P complexs that special molecular structure is arranged, and are a kind of new and effective antioxidants, are the most potent free-radical scavengerss of finding so far.The Green Tea Extract oxidation capacity that experiment showed, OPC is 50 times of vitamin-E, ascorbic 20 times, is generally the reddish-brown powder, little, the puckery of gas, water-soluble and most organic solvent.Because its phenolic hydroxyl group group number is many, so it is strong to remove the free radical ability.
Flavones extensively exists in natural certain plants and the berry, the nearly kind more than 4,000 of sum, and its molecular structure is not quite similar, the effect of flavones is many-sided, it is a kind of very strong oxidation inhibitor, can effectively remove free radical, and the ability of this prevention oxidation is more than 10 times of vitamin-E.
So tannin (Tannins) is complicated polyhydric phenols, because can be used for tanning skin the tannin of gaining the name.Be distributed widely in vegitabilia, more general to distribute in the higher plant especially, as in garden burnet, pomegranate rind, giant knotweed, folium ilicis chinensis, arbor-vitae, Herba Agrimoniae, the sophora bud, the rheum officinale etc. a large amount of existence being arranged all.It also is a kind of very strong oxidation inhibitor, can effectively remove free radical.
The polyphenolic compound that the present invention adopts and can effectively remove free radical, avoids causing free chain reaction is added in the PG cutting liquid, because polyphenolic compound can water-soluble and most organic solvent, thereby has intermiscibility preferably with PG.When grinding top layer in the cutting process forms higher thermograde (＞300 ℃), scission reaction can take place in the part PG that contacts with the grinding top layer, polyphenolic compound can be in time with the free radical reaction of cracking generation and with its removing, avoid causing other PG molecule generation free radical chain reactions, thereby play the effect of stablizing the PG moiety.
The invention provides a kind of diamond wire cutting liquid and preparation method thereof, its beneficial effect is as follows:
1, in the traditional multi-thread cutting process, because the grinding top layer forms higher thermograde (＞300 ℃), causes the part PG that contacts with the grinding top layer that scission reaction can take place, thereby the PG moiety is changed; The present invention adopts polyphenolic compound to be added in the PG cutting liquid and can in time dispose with the free radical reaction of cracking generation and with it, avoid causing other PG molecule generation free radical chain reactions, stablize the PG molecular structure, keep the constant substantially effect of PG relative molecular mass thereby play;
2, PG moiety variable effect PG cuts liquid cooling but property and oilness in the cutting liquid, and cutting liquid cooling and oilness have bigger influence to yield rate in the diamond wire cutting silicon chip process; By the utilization of the technology of the present invention, can increase PG cutting liquid and reuse number of times, strengthen the usage quantity that reclaims liquid in the multi-thread cutting process, and finally reach the purpose that reduces the silicon chip cutting cost;
3, polyphenolic compound used in the present invention has good infiltration, lubrication, has obviously reduced surface damage, mechanical stress and the thermal stresses of section, has increased the yield rate of silicon chip;
4, the present invention is applied widely, can effectively be suitable for to the cutting of lines such as silicon single crystal, polysilicon, and can significantly improve the utilization ratio of above-mentioned diamond wire cutting liquid;
5, the present invention has solved the problem that the diamond wire cutting liquid uses later stage smear metal and pelletizing powder to deposit again effectively, has avoided the chemical bonding-adsorption of silicon chip surface, is convenient to cleaning and the following process of silicon chip;
6, the whole comprehensive treating process of the present invention and to utilize the process of silicon chip smear metal mortar be the combination of physics, chemistry is an environmentally friendly technology system, and cleaning, safety, pollution are little;
7, in process of production, smear metal liquid all can consume resources such as a large amount of electric power, water, by the recovery technology of this invention, the use that moves in circles can energy efficient, improves service efficiency, bring considerable economic benefit for a large amount of silicon chip cutting enterprise, obtain bigger social benefit simultaneously.
Embodiment
Embodiment one
A kind of diamond wire cutting liquid, it contains propylene glycol cutting liquid, also contains polyphenolic compound pycnogenols (Powdered), and its weight percent in propylene glycol cutting liquid is 0.1%.
Embodiment two
A kind of diamond wire cutting liquid, it contains propylene glycol cutting liquid, also contains polyphenolic compound tannin (Powdered), and its weight percent in propylene glycol cutting liquid is 0.1%.
Embodiment three
A kind of diamond wire cutting liquid, it contains propylene glycol cutting liquid, also contains polyphenolic compound flavones (Powdered), and its weight percent in propylene glycol cutting liquid is 0.1%.
Embodiment four
Pycnogenols (Powdered) is added in the PG cutting liquid with 0.1% weight percent, fully stirs 0.5h and make it to be dissolved in the PG cutting liquid, realized the preparation of diamond wire cutting liquid.
Embodiment five
Tannin (Powdered) is added in the PG cutting liquid with 0.1% weight percent, fully stirs 0.5h and make it to be dissolved in the PG cutting liquid, realized the preparation of diamond wire cutting liquid.
Embodiment six
Flavones (Powdered) is added in the PG cutting liquid with 0.1% weight percent, fully stirs 0.5h and make it to be dissolved in the PG cutting liquid, realized the preparation of diamond wire cutting liquid.
Embodiment seven
Pycnogenols (Powdered) is added in the PG cutting liquid with 5.0% weight percent, fully stirs 0.5h and make it to be dissolved in the PG cutting liquid, realized the preparation of diamond wire cutting liquid.
Embodiment eight
Tannin (Powdered) is added in the PG cutting liquid with 5.0% weight percent, fully stirs 0.5h and make it to be dissolved in the PG cutting liquid, realized the preparation of diamond wire cutting liquid.
Embodiment nine
Flavones (Powdered) is added in the PG cutting liquid with 5.0% weight percent, fully stirs 0.5h and make it to be dissolved in the PG cutting liquid, realized the preparation of diamond wire cutting liquid.
Embodiment ten
Pycnogenols (Powdered) is added in the PG cutting liquid with 0.5% weight percent, fully stirs 0.5h and make it to be dissolved in the PG cutting liquid, realized the preparation of diamond wire cutting liquid.
Embodiment 11
Tannin (Powdered) is added in the PG cutting liquid with 0.5% weight percent, fully stirs 0.5h and make it to be dissolved in the PG cutting liquid, realized the preparation of diamond wire cutting liquid.
Embodiment 12
Flavones (Powdered) is added in the PG cutting liquid with 0.5% weight percent, fully stirs 0.5h and make it to be dissolved in the PG cutting liquid, realized the preparation of diamond wire cutting liquid.
Effect embodiment
For the checking explanation being provided for beneficial effect of the present invention, now embodiment 6,7,10 diamond wire cutting liquid are used for the silicon chip cutting experiment, the application conditions of cutting condition and commercially available cutting liquid is consistent, and reclaim cutting the waste liquid that the back produces, contrast the difference between commercially available cutting liquid and the diamond wire cutting liquid, correlation data is as follows as a result for the molecular weight variation of cutting liquid and silicon chip cutting:
Table 1: cutting liquid mean molecule changes relatively
| Cutting liquid title | New liquid molecular-weight average | The liquid molecular-weight average is reclaimed in the cutting back |
| Commercially available propylene glycol cutting liquid | 75～80 | 65～70 |
| Embodiment 1 cutting liquid | 76～82 | 75～81 |
Table 2: dirty sheet rate, stria sheet rate, yield rate be (cutting for the first time) relatively
| Cutting liquid title | Dirty sheet rate (%) | Stria sheet rate (%) | Yield rate (%) |
| Commercially available propylene glycol cutting liquid | 1.0 | 0.1 | 95.0 |
| Embodiment 1 cutting liquid | 0.9 | 0.1 | 95.3 |
Table 3: dirty sheet rate, stria sheet rate, yield rate be (cutting for the second time) relatively
| Cutting liquid title | Dirty sheet rate (%) | Stria sheet rate (%) | Yield rate (%) |
| Commercially available propylene glycol cutting liquid | 2.1 | 0.8 | 90.6 |
| Embodiment 1 cutting liquid | 1.1 | 0.2 | 94.7 |
By above-mentioned test as can be known, silicon carbide cutting liquid of the present invention effectively reduces the dirty sheet rate of silicon chip, has improved the yield rate of silicon chip.
In addition, find in the composition by the regenerated liquid component that from waste slurry, reclaims: obviously have light constituent to increase after the commercially available cutting liquid that does not add polyphenolic compound reclaims, and the basic no change of diamond wire cutting liquid of the present invention component after reclaiming, illustrate that commercially available cutting liquid has chain rupture to take place in cutting process, and chain rupture does not take place in diamond wire cutting liquid of the present invention, can effectively guarantee to cut the quality that liquid reclaims, increase recovered frequency, reduce cutting cost.
Above is detailed description of the invention in conjunction with embodiment; only be explanation technical conceive of the present invention and characteristics; its purpose is to allow the people that is familiar with this technology understand content of the present invention and is implemented; can not limit protection scope of the present invention with this; all equivalences that spirit is done according to the present invention change or modify, and all should be encompassed in protection scope of the present invention.
Claims (4)
1. diamond wire cutting liquid, contain propylene glycol cutting liquid, it is characterized in that, also contain polyphenolic compound, described polyphenolic compound is one or more in pycnogenols class, flavonoid, tannins, phenolic acids, the anthocyanin class, and the weight percent of described polyphenolic compound in propylene glycol cutting liquid is 0.1%～5.0%.
2. cutting liquid according to claim 1 is characterized in that, described polyphenolic compound is Powdered.
3. the preparation method of a diamond wire cutting liquid is characterized in that may further comprise the steps:
(1) each component weighing: polyphenolic compound and propylene glycol cutting liquid are carried out weighing respectively;
(2) preparation diamond wire cutting liquid: get institute's weighing in the step (1) polyphenolic compound, be added in the propylene glycol cutting liquid, fully stir dissolving down, make the diamond wire cutting liquid;
The weight percent of polyphenolic compound in propylene glycol cutting liquid is 0.1%～5.0% in the step (1).
4. preparation method according to claim 3 is characterized in that, when fully stirring in the step (2), churning time is 0.5～1 hour.
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| CN 201110325955 CN102433190B (en) | 2011-10-24 | 2011-10-24 | Diamond linear cutting fluid and preparation method thereof |
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| CN 201110325955 CN102433190B (en) | 2011-10-24 | 2011-10-24 | Diamond linear cutting fluid and preparation method thereof |
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| CN102433190A CN102433190A (en) | 2012-05-02 |
| CN102433190B true CN102433190B (en) | 2013-08-07 |
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