CN103396875A - Cooling liquid for diamond-wire cutting equipment, and preparation method thereof - Google Patents
Cooling liquid for diamond-wire cutting equipment, and preparation method thereof Download PDFInfo
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- CN103396875A CN103396875A CN201310335944XA CN201310335944A CN103396875A CN 103396875 A CN103396875 A CN 103396875A CN 201310335944X A CN201310335944X A CN 201310335944XA CN 201310335944 A CN201310335944 A CN 201310335944A CN 103396875 A CN103396875 A CN 103396875A
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Abstract
The invention provides a cooling liquid for diamond-wire cutting equipment, and a preparation method thereof. The cooling liquid consists of: 2.5 wt%-90 wt% of deionized water, 2 wt%-86 wt% of diethylene glycol, 0.1 wt%-10 wt% of polyethylene glycol with an average molecular weight of 100-2000, 1 wt% -30 wt% of a dispersant, 0.01 wt% -10 wt% of a chelating agent, 0.1 wt% -10 wt% of a metal corrosion inhibitor and 0.01 wt% -5 wt% of an antifoaming agent. The preparation method comprises: successively adding the chelating agent, the metal corrosion inhibitor and the antifoaming agent into deionized water according to the ratio, uniformly stirring; and then adding diethylene glycol, the dispersant and polyethylene glycol, stirring for 6-8 hours to prepare the cooling liquid for the diamond-wire cutting equipment. The cooling liquid for the diamond-wire cutting equipment has the characteristics of good cooling effect, moderate silicon-powder suspension capability, low viscosity, few foams and low corrosivity, and is simple in manufacture and low in cost.
Description
Technical field
The present invention relates to the cooling fluid of using in the silicon wafer cutting technique, be specifically related to a kind of cooling fluid for diamond wire saw silicon single crystal.
Background technology
The material that present solar-energy photo-voltaic cell uses mainly contains non-crystalline silicon, polysilicon, silicon single crystal, III-V family multi-element compounds etc.Wherein silicon single crystal has the high light photoelectric transformation efficiency, and material itself does not pollute environment, the characteristics such as material source is extensive, stable performance.In the monocrystalline silicon battery manufacturing processed, the silicon single crystal rod of vertical pulling need to be cut into the silicon chip of thickness in the 200um left and right.
The main dual mode that adopts cuts now: mortar multi-wire saw and diamond wire multi-wire saw.Diamond wire saw is compared mortar cutting, and to have a cutting efficiency high, low cost, and low the pollution, the characteristics that quality is higher, more meet the needs of Sustainable development, compares traditional mortar cutting and have more competitive edge.When using diamond wire saw, need to spray on line cooling fluid, reduce on the one hand the temperature of cutting seam, can lubricate diamond wire on the other hand, take away and silica flour that Effective Suspension cuts down.
Present existing diamond wire cooling fluid mainly is divided into following three kinds: a kind of is the cooling fluid of polyethylene glycol system, a kind of Special cutting fluid for diamond wire is disclosed in Chinese invention patent application prospectus CN102352278A, it is mainly take polyoxyethylene glycol as main, add a certain proportion of rust-preventive agent, emulsifying agent and defoamer, this cooling fluid advantage is that cooling performance is better, for impurity such as silica flours, certain suspension and sequestering action are arranged, because its Polyethylene glycol is 19wt%～59wt%(weight percent), make its cost higher.For simplicity, below " wt%(weight percent) " is abbreviated as " wt% ".
A kind of is small molecular alcohol, ether, phenols combination cooling liquid, a kind of diamond linear cutting fluid and preparation method thereof is disclosed in Chinese invention patent application prospectus CN102433190A, it is mainly take propylene glycol as main body, by adding other ethers and the formulated cooling fluid of phenols additive, the advantage of this cooling fluid is that the performance to silicon chip surface has some improvement, cost is relatively low, but that its shortcoming is cooling performance is general, for the dispersion effect of the impurity such as silica flour, is not very desirable.
A kind of is water base cooling fluid, mainly take water as main, by a kind of cooling fluid that adds dispersion agent, sequestrant, tensio-active agent, defoamer and viscosity modifier to form, this cooling fluid cost is low, environmental friendliness, but the problem that will solve is exactly how to disperse the impurity such as silica flour.
The cooling fluid of existing market in use has following problem usually: (1) cooling performance is not good.The silicon ingot temperature is elevated to more than 30 ℃ in cutting process, and except the generation section was bad, also easily softening bar glue, made sheet, fall rod, brings about great losses.(2) very good or too poor to the suspension of silica flour.Suspension is very good, makes silica flour easier of cooling fluid enters joint-cutting repeatedly, reduces the cutting efficiency of diamond wire, also more easily forms TTV bad; Suspension is too poor, makes silica flour easily be deposited in each corner, the especially plate-type heat exchanger of equipment, makes cooling fluid and process cooling water heat exchange bad, can not effectively reduce coolant temperature, causes cutting bad.(3) easily produce bubble when recycling.In cutting process, a large amount of bubbles are present in the surface of diamond wire, make the cooling cooling fluid with suspension of actual participation reduce in a large number, cause the silicon chip surface temperature distributing disproportionation, easily produce fragment, stria etc. bad.(4) the acid cooling fluid of part is easily corroded steel wire.Make diamond not firm in the steel wire surface bonding, easily come off, can not give full play to the cutting power of diamond wire, What is more reduces the tensile strength of steel wire, easily produces broken string.
Cooling fluid is one of important auxiliary material of diamond wire saw, accounts for the 23wt% of its auxiliary material cost, accounts for the 11wt% of manufacturing cost.Its most of product is imported product, and price is high,, in order further to realize reducing costs cleaner production, improves cutting quality, needs a kind of cooling fluid of new production domesticization to meet diamond wire saw silicon single crystal.
Summary of the invention
Goal of the invention of the present invention: the shortcoming that the present invention exists in order to overcome above-mentioned prior art, provide a kind of and have simultaneously that good cooling results, silica flour suspending power are moderate, the cooling fluid of low viscosity, low foam, low-corrosiveness, and the preparation method of this cooling fluid.
Technical scheme of the present invention is: a kind of cooling fluid for diamond wire saw equipment, it mainly is comprised of the Diethylene Glycol of 2.5wt%～90wt% deionized water, 2wt%～86wt%, the polyoxyethylene glycol of 0.1wt%～10wt%, the dispersion agent of 1wt%～30wt%, the sequestrant of 0.01wt%～10wt%, the metal corrosion inhibitor of 0.1wt%～10wt%, the defoamer of 0.01wt%～5wt%, and described polyoxyethylene glycol molecular-weight average is 100～2000.
A preferred version as a kind of cooling fluid for diamond wire saw equipment of the present invention, the cooling fluid of diamond wire saw equipment mainly is comprised of the polyoxyethylene glycol of 2.5wt%～80wt% deionized water, 0.1wt%～5wt%, the dispersion agent of 5wt%～25wt%, the Diethylene Glycol of 10wt%～80wt%, the sequestrant of 0.01wt%～5wt%, the metal corrosion inhibitor of 1wt%～5wt%, the defoamer of 0.01wt%～3wt%, and described polyoxyethylene glycol molecular-weight average is 100～1000.
As more preferably scheme, the cooling fluid of diamond wire saw equipment mainly is comprised of the deionized water of 2.5wt%～57.88wt%, the polyoxyethylene glycol of 0.1wt%～1wt%, the dispersion agent of 10wt%～20wt%, the Diethylene Glycol of 30wt%～70wt%, the sequestrant of 0.01wt%～2wt%, the metal corrosion inhibitor of 2wt%～4wt%, the defoamer of 0.01wt%～0.5wt%, and described polyoxyethylene glycol molecular-weight average is 100～600.
As scheme most preferably, the cooling fluid of diamond wire saw equipment mainly is comprised of the deionized water of 28.5wt%～47.88wt%, the polyoxyethylene glycol of 0.1wt%～1wt%, the dispersion agent of 10wt%～20wt%, the Diethylene Glycol of 40wt%～45wt%, the sequestrant of 0.01wt%～2wt%, the metal corrosion inhibitor of 2wt%～4wt%, the defoamer of 0.01wt%～0.5wt%, and described polyoxyethylene glycol molecular-weight average is 100～600.
Described dispersion agent is by one or more in vinylformic acid, methacrylic acid, ethylacrylic acid, olefin sulfonic acid, styrene sulfonic acid, maleic anhydride, alkyl propenyloxy group sulfonic acid, acrylamido sulfonic acid, ethylene glycol, Diethylene Glycol, ethylene glycol monomethyl ether, ethylene glycol ethyl ether, oxyethane, monomeric unit and the homopolymer that obtains or one or more in multipolymer;
Described sequestrant is comprised of one or more in hydramine, polyamines base organic amine or amino acid.
Described metal corrosion inhibitor is comprised of one or more in alcamines, phenols, carboxylic-acid, carboxylic acid lipid, anhydrides, benzotriazole and Sodium Nitrite.
Described defoamer is one or more in polymethyl siloxane, organo-siloxane, polyethers.
A kind of preparation method of the cooling fluid for diamond wire saw equipment:
(1) sequestrant, metal corrosion inhibitor and defoamer are added in deionized water by proportioning, stir;
(2) Diethylene Glycol, dispersion agent and polyoxyethylene glycol are added step (1) gained solution, then stir and obtained described cooling fluid for diamond wire saw equipment in 6-8 hour.
The effect of each component in the present invention:
Defoamer: surface tension is little, and surfactivity is high, has the froth breaking ability, and in cutting process, because cooling fluid circulates in equipment, cooling fluid own is again the mixture of organism and water, easily produces bubble.This bubble can make the cutting thermal conductance go out inequality, the silica flour dispersion is uneven, causes cutting bad.
Polyoxyethylene glycol: can be water-soluble, reduce by the frictional force between diamond wire, diamond and silicon chip, play the effect of lubrication.
Dispersion agent: in cutting process, can produce the impurity such as a large amount of silica flours, iron and diamond, therefore need to select suitable dispersion agent to disperse silica flour, improve the silicon chip surface quality.
Diethylene Glycol: not only good at the hot conditions stability inferior, can be good at playing the effect of lubrication and cooling, and silica flour is also had certain dispersive ability.
Sequestrant and metal corrosion inhibitor:, because cooling fluid flows in the board pipeline, by diamond wire, carried and entered joint-cutting, it all can have certain corrosive nature for pipeline, diamond steel wire, therefore must add sequestrant to suppress the generation of corrosion.
A kind of the key technical indexes of cooling fluid for diamond wire saw equipment of the present invention is: specific heat is greater than 4kJ/kg. ℃, viscosity 5～15cp, density 1.05～1.15g/cm
3, pH value 5.5～7, specific conductivity is less than 200us/cm.
The invention has the beneficial effects as follows: (1) cooling fluid for diamond wire saw silicon single crystal of the present invention has that good cooling results, silica flour suspending power are moderate, the cooling fluid of low viscosity, low foam, low-corrosiveness; (2) cooling fluid for diamond wire saw silicon single crystal of the present invention is with low cost, makes simple.
Embodiment
A kind of cooling fluid for diamond wire saw equipment, mainly the Diethylene Glycol of 2.5wt%～90wt% deionized water, 2wt%～86wt%, the polyoxyethylene glycol of 0.1wt%～10wt%, the dispersion agent of 1wt%～30wt%, the sequestrant of 0.01wt%～10wt%, the metal corrosion inhibitor of 0.1wt%～10wt%, the defoamer of 0.01wt%～5wt%, consist of, described polyoxyethylene glycol molecular-weight average is 100～2000.
Further, a kind of cooling fluid for diamond wire saw equipment, mainly the polyoxyethylene glycol of 2.5wt%～80wt% deionized water, 0.1wt%～5wt%, the dispersion agent of 5wt%～25wt%, the Diethylene Glycol of 10wt%～80wt%, the sequestrant of 0.01wt%～5wt%, the metal corrosion inhibitor of 1wt%～5wt%, the defoamer of 0.01wt%～3wt%, consist of, described polyoxyethylene glycol molecular-weight average is 100～1000.
As more preferably scheme, the cooling fluid of diamond wire saw equipment, mainly the deionized water of 2.5wt%～57.88wt%, the polyoxyethylene glycol of 0.1wt%～1wt%, the dispersion agent of 10wt%～20wt%, the Diethylene Glycol of 30wt%～70wt%, the sequestrant of 0.01wt%～2wt%, the metal corrosion inhibitor of 2wt%～4wt%, the defoamer of 0.01wt%～0.5wt%, consist of, described polyoxyethylene glycol molecular-weight average is 100～600.
As scheme most preferably, the cooling fluid of diamond wire saw equipment mainly is comprised of the deionized water of 28.5wt%～47.88wt%, the polyoxyethylene glycol of 0.1wt%～1wt%, the dispersion agent of 10wt%～20wt%, the Diethylene Glycol of 40wt%～45wt%, the sequestrant of 0.01wt%～2wt%, the metal corrosion inhibitor of 2wt%～4wt%, the defoamer of 0.01wt%～0.5wt%, and described polyoxyethylene glycol molecular-weight average is 100～600.
The composition proposal of described dispersion agent is: by the mixing of one or more materials of one or more monomeric units in vinylformic acid, methacrylic acid, ethylacrylic acid, olefin sulfonic acid, styrene sulfonic acid, maleic anhydride, alkyl propenyloxy group sulfonic acid, acrylamido sulfonic acid, ethylene glycol, Diethylene Glycol, ethylene glycol monomethyl ether, ethylene glycol ethyl ether, oxyethane in the material that homopolymerization or copolymerization obtain; Preferred version is: the mixing of one or more materials of one or more monomeric units in ethylene glycol, Diethylene Glycol, ethylene glycol monomethyl ether, ethylene glycol ethyl ether, oxyethane in the material that homopolymerization or copolymerization obtain.Most preferably scheme is: the mixing of one or more materials of one or more monomeric units in Diethylene Glycol, ethylene glycol monomethyl ether, oxyethane in the material that homopolymerization or copolymerization obtain.
The composition proposal of described sequestrant is: the mixing of one or more in diethanolamine, trolamine, ethylenediamine tetraacetic acid (EDTA), polyamines base organic amine or amino acid; Preferred version is: the mixing of one or more in trolamine, ethylenediamine tetraacetic acid (EDTA); Most preferred scheme is: ethylenediamine tetraacetic acid (EDTA).
The composition proposal of described metal corrosion inhibitor is: the mixing of one or more in alcamines (as: diethanolamine, trolamine), phenols (as: phenol, pyrocatechol), carboxylic-acid (as: para-amino benzoic acid, Whitfield's ointment, citric acid), carboxylic acid lipid (as: benzaminic acid, methyl benzoate, Methyl Benzene-o-dicarboxylate), anhydrides (as: diacetyl oxide), benzotriazole and Sodium Nitrite; Preferred version is: the mixing of one or more in trolamine, benzotriazole and Sodium Nitrite; Most preferred scheme is: benzotriazole.
The composition proposal of described defoamer is: the mixing of one or more in polymethyl siloxane, organo-siloxane, polyethers; Preferred version is: the mixing of one or more of organo-siloxane, polyethers; Most preferred scheme is: organo-siloxane.
The present invention is described further below in conjunction with example, and in embodiment, the proportioning of each component is as shown in table 1.
Table 1 embodiment component
Above-described embodiment is carried out the measurement of relevant physical properties, all embodiment all meet: specific heat is greater than 4kJ/kg. ℃, and viscosity is in the 5-15cp scope, and density is at 1.05-1.15g/cm
3In scope, pH value is in the 5.5-7 scope, and specific conductivity is less than 200us/cm.
In described embodiment 1,10,11:
Dispersion agent: select the mixing through the homopolymerization material of vinylformic acid, olefin sulfonic acid, maleic anhydride, ethylene glycol, ethylene glycol monomethyl ether, ethylene glycol ethyl ether, oxyethane;
Metal corrosion inhibitor: select the mixture thing in phenol, para-amino benzoic acid, benzaminic acid, methyl benzoate, diacetyl oxide;
Sequestrant: select diethanolamine, trolamine, ethylenediamine tetraacetic acid (EDTA), polyamines base organic amine or amino acid whose mixture;
Defoamer: select the mixture in polymethyl siloxane, organo-siloxane, polyethers.
In described embodiment 2,8,9:
Dispersion agent: the mixture that obtains material in ethylene glycol, ethylene glycol monomethyl ether, oxyethane through copolymerization;
Metal corrosion inhibitor: the mixture of trolamine, benzotriazole and Sodium Nitrite;
Sequestrant: the mixture of selecting trolamine, ethylenediamine tetraacetic acid (EDTA);
Defoamer: the mixture of selecting organo-siloxane, polyethers.
In described embodiment 3-7:
Dispersion agent: select to obtain the mixture of material through homopolymerization in Diethylene Glycol, ethylene glycol monomethyl ether, oxyethane;
Metal corrosion inhibitor: select benzotriazole;
Sequestrant: select ethylenediamine tetraacetic acid (EDTA);
Defoamer: select organo-siloxane.
Embodiment is carried out performance index to be detected, mainly comprise dispersiveness to silica flour, Corrosion of Stainless Steel inhibition, the detection that forms foam height and cutting yield are detected the (silica flour that adds 20wt% in cooling fluid, sedimentation one Zhou Houzai shakes up again, detect dispersiveness and the redispersibility of cooling fluid to silica flour, use the Luo Shi Latherometer to detect the cooling fluid foam height), detected result is as shown in table 2:
Table 2 performance index
Can find out based on the embodiments of the invention performance and be better than existing cooling fluid comprehensively from the data of table 2, its proportioning is with low cost, collocation method is simple, through found that experimental test draws, its indices of cooling fluid of the present invention all can meet the requirement of existing installation and method, and can improve the loss of its good article rate and reduction equipment.
A kind of preparation method of the cooling fluid for diamond wire saw equipment, comprise the steps:
(1) sequestrant, metal corrosion inhibitor and defoamer are added in deionized water by proportioning, stir;
(2) Diethylene Glycol, dispersion agent and polyoxyethylene glycol are added step (1) gained solution, then stir and obtained described a kind of cooling fluid for diamond wire saw equipment in 6-8 hour.
Should be understood that; for those skilled in the art; under the premise without departing from the principles of the invention; can also make some improvements and modifications; these improvements and modifications also should be considered as protection scope of the present invention, in the present embodiment not clear and definite each integral part all available prior art realized.
Claims (9)
1. cooling fluid that is used for diamond wire saw equipment, it is characterized in that: it mainly is comprised of the Diethylene Glycol of 2.5wt%～90wt% deionized water, 2wt%～86wt%, the polyoxyethylene glycol of 0.1wt%～10wt%, the dispersion agent of 1wt%～30wt%, the sequestrant of 0.01wt%～10wt%, the metal corrosion inhibitor of 0.1wt%～10wt%, the defoamer of 0.01wt%～5wt%, and described polyoxyethylene glycol molecular-weight average is 100～2000.
2. a kind of cooling fluid for diamond wire saw equipment according to claim 1, it is characterized in that: the cooling fluid of diamond wire saw equipment mainly is comprised of the Diethylene Glycol of 2.5wt%～80wt% deionized water, 10wt%～80wt%, the polyoxyethylene glycol of 0.1wt%～5wt%, the dispersion agent of 5wt%～25wt%, the sequestrant of 0.01wt%～5wt%, the metal corrosion inhibitor of 1wt%～5wt%, the defoamer of 0.01wt%～3wt%, and described polyoxyethylene glycol molecular-weight average is 100～1000.
3. a kind of cooling fluid for diamond wire saw equipment according to claim 2, it is characterized in that: the cooling fluid of diamond wire saw equipment mainly is comprised of the deionized water of 2.5wt%～57.88wt%, the Diethylene Glycol of 30wt%～70wt%, the polyoxyethylene glycol of 0.1wt%～1wt%, the dispersion agent of 10wt%～20wt%, the sequestrant of 0.01wt%～2wt%, the metal corrosion inhibitor of 2wt%～4wt%, the defoamer of 0.01wt%～0.5wt%, and described polyoxyethylene glycol molecular-weight average is 100～600.
4. a kind of cooling fluid for diamond wire saw equipment according to claim 3, it is characterized in that: the cooling fluid of diamond wire saw equipment mainly is comprised of the deionized water of 28.5wt%～47.88wt%, the polyoxyethylene glycol of 0.1wt%～1wt%, the Diethylene Glycol of 40wt%～45wt%, the dispersion agent of 10wt%～20wt%, the sequestrant of 0.01wt%～2wt%, the metal corrosion inhibitor of 2wt%～4wt%, the defoamer of 0.01wt%～0.5wt%, and described polyoxyethylene glycol molecular-weight average is 100～600.
5. according to claim 1,2,3 or 4 described a kind of cooling fluids for diamond wire saw equipment, it is characterized in that: described dispersion agent is the mixing of one or more materials of one or more monomeric units in the material that homopolymerization or copolymerization obtain in vinylformic acid, methacrylic acid, ethylacrylic acid, olefin sulfonic acid, styrene sulfonic acid, maleic anhydride, alkyl propenyloxy group sulfonic acid, acrylamido sulfonic acid, ethylene glycol, Diethylene Glycol, ethylene glycol monomethyl ether, ethylene glycol ethyl ether, oxyethane.
6. according to claim 1,2,3 or 4 described a kind of cooling fluids for diamond wire saw equipment, it is characterized in that: described sequestrant is one or more the mixing in diethanolamine, trolamine, ethylenediamine tetraacetic acid (EDTA), polyamines base organic amine or amino acid.
7. according to claim 1,2,3 or 4 described a kind of cooling fluids for diamond wire saw equipment, it is characterized in that: described metal corrosion inhibitor is one or more the mixing in alcamines, phenols, carboxylic-acid, carboxylic acid lipid, anhydrides, benzotriazole and Sodium Nitrite.
8. according to claim 1,2,3 or 4 described a kind of cooling fluids for diamond wire saw equipment, it is characterized in that: described defoamer is one or more the mixing in polymethyl siloxane, organo-siloxane, polyethers.
9. according to claim 1, the preparation method of 2,3 or 4 described a kind of cooling fluids for diamond wire saw equipment, comprise the steps:
(1) sequestrant, metal corrosion inhibitor and defoamer are added in deionized water by proportioning, stir;
(2) Diethylene Glycol, dispersion agent and polyoxyethylene glycol are added step (1) gained solution, then stir and obtained described cooling fluid for diamond wire saw equipment in 6-8 hour.
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