CN112111320B - Oil composition for cutting polycrystalline silicon, preparation method and application thereof - Google Patents
Oil composition for cutting polycrystalline silicon, preparation method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/048—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution, non-macromolecular and macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
- C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/02—Hydroxy compounds
- C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
- C10M2207/026—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with tertiary alkyl groups
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/40—Fatty vegetable or animal oils
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
- C10M2215/064—Di- and triaryl amines
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The invention relates to a polycrystalline silicon cutting oil composition, a preparation method and application thereof, and mainly solves the problems of poor low-temperature continuous stability, easy putrefaction of water-based products, corrosion risk to equipment and poor universality of various materials in the prior art. 85-97% of low-viscosity base oil, 2-15% of lubricating dispersant, 0.1-1% of oleic acid and 0.4-1% of antioxidant; the preparation method comprises the following steps: 1-2 kinds of low-viscosity base oil is added into a blending kettle and uniformly stirred, other additives are added according to the weight percentage, and the mixture is stirred for more than 1 hour at normal temperature or at the temperature of 40-50 ℃ for 20-30 min until the mixture is uniform and transparent.
Description
Technical Field
The invention relates to an oil composition for cutting polycrystalline silicon, a preparation method and application thereof.
Background
In the cutting process of some polycrystalline silicon wires, carborundum added into cutting liquid is required to be well suspended in the cutting liquid, and when the carborundum is sprayed on the cutting wire which is moved away quickly, the carborundum can have good permeability and adhesive force on the cutting wire so as to ensure that the outer layer of the cutting wire is uniformly wrapped with enough carborundum, finally the cutting wire is kept in a lasting sharp state and is effectively rubbed with a cut silicon wafer for a long time, and the processing efficiency is ensured; in addition, after the polycrystalline silicon is cut, the roughness and the qualification rate of the cut surface are ensured, and the problem of large deviation and the like caused by incontrollable fragmentation can not be presented; the foam is small during processing to reduce or eliminate the negative impact on the cutting effect during processing. At present, carborundum cutting fluid for cutting nonmetal brittle and hard materials such as polycrystalline silicon and the like is mainly a water-based product, such as ethylene glycol and aqueous solution; or water and various surfactants, polyethylene glycol compositions and the like, has poor penetration and spreading properties compared with the light oil, is easy to foam when used, and needs to introduce a defoaming agent properly for foam inhibition; in addition, since the paint needs to be diluted with a large amount of water for use, there is a risk of corrosion of the equipment.
The patent CN107325875A is characterized in that the carborundum wire cutting fluid consists of the following components: fatty alcohol, polypropylene glycol, polyoxyethylene, polyoxypropylene ether, an organic silicon defoaming agent and distilled water. The problems that the surface of a silicon wafer cut by the existing carborundum cutting fluid has large TTV, line marks and low cleanliness are mainly solved.
The patent CN103184094A cooling liquid mainly comprises a lubricant, an emulsifier, an antirust agent, a dispersant, a preservative and deionized water, wherein the mass percentages of the components are as follows: 5 to 50 percent of lubricant, 0.05 to 10 percent of emulsifier, 0.1 to 5 percent of antirust agent, 0 to 10 percent of dispersant, 0 to 5 percent of preservative, and the balance of deionized water. The cooling liquid has excellent lubricity, dispersibility and easy cleaning property, is suitable for cutting hard and brittle materials such as crystalline silicon, sapphire and the like, and can ensure the surface smoothness of slices while being used for high-speed cutting of diamond wires so as to improve the product percent of pass.
Patent CN104395448a discloses a water-soluble working fluid for use in cutting a brittle material with a wire saw, which is capable of suppressing the bending of a wire and obtaining a good cutting accuracy when cutting a brittle material with a saw wire having a fine wire diameter by selecting a water-soluble polymer compound having an average molecular weight of 3 × 103 or more and 6 × 105 or less.
While the above patents are mainly water-based cutting fluid products, diamond wire cutting fluids are described in terms of cutting accuracy, dispersibility and the like of chips, and some of them also use defoaming agents and emulsifiers to improve permeability and defoaming capability. However, the low-temperature environment operation performance is stable, the corrosion resistance is not easy to decay, and the corrosion resistance of various materials is not described, so that a product with excellent comprehensive stability is needed at present.
Disclosure of Invention
The invention aims to solve the technical problems that in the prior art, the low-temperature continuous stability is poor, a water-based product is easy to decay, the equipment is corroded, and the universality of various materials is poor, and provides a novel oil composition for cutting polycrystalline silicon, which is combined by an oil formula, so that carborundum can continuously and well keep the dispersity in a cutting fluid, effectively permeate and adhere to a cutting line for a long time, and keep higher processing efficiency. The formula is not water-soluble processing liquid, water is not required to be added for use, and a defoaming agent or a surfactant is not required to be added, so that the good wettability can be ensured, the foaming tendency is avoided, the environmental persistence performance is more stable, the corrosion risk and the corruption are avoided, and the like, and the method can be used for processing general cutting and grinding of non-metal materials such as polycrystalline silicon and optical glass and metal materials, and has the advantage of strong universality. The second technical problem to be solved by the present invention is to provide a method for preparing an oil composition for cutting polycrystalline silicon, which corresponds to the first technical problem. The present invention is also directed to a use of the composition for solving the above-mentioned problems.
In order to solve the first technical problem, the technical scheme adopted by the invention is as follows: an oil composition for cutting polycrystalline silicon comprises the following components in percentage by weight: 85-97% of low-viscosity base oil, 2-7% of lubricating dispersant, 0.1-1% of oleic acid and 0.4-1% of antioxidant.
In the above technical solution, preferably, the components further include, by weight: 0.01 to 0.08 percent of odor improver.
In the above technical scheme, preferably, the kinematic viscosity range of the low-viscosity base oil at 40 ℃ is 1.5-7.0 mm 2 and/S, the low-viscosity base oil is at least one selected from light white oil or oil for L-AN 5 total loss system, isomeric hydrocarbon solvent oil or low-viscosity PAO hydrogenated polydecene.
In the above technical solution, preferably, the lubricant dispersant is selected from oxidized vegetable oil, isomeric vegetable oil, and branched vegetable oilAt least one of a chain polymer ester or a high molecular weight complex ester having a kinematic viscosity of 35 to 350mm at 100 DEG C 2 /S。
In the above technical solution, preferably, the antioxidant is at least one selected from hindered phenol antioxidants and aromatic amine antioxidants.
In the above technical solution, preferably, the hindered phenol antioxidant is selected from at least one of monophenol, alkyl polyphenol, and thiobisphenol; the aromatic amine antioxidant is at least one of diarylsecondary amine or p-phenylenediamine.
In the above technical solution, preferably, the odor improver is at least one selected from a group consisting of ice orange essence and rose essence.
To solve the second technical problem, the invention adopts the following technical scheme:
the preparation method of the oil composition for cutting polycrystalline silicon comprises the following preparation steps: adding the low-viscosity base oil into a blending kettle, uniformly stirring, adding other additives according to the weight percentage, and stirring at normal temperature for 50-80 min or at 40-50 ℃ for 20-30 min until the mixture is uniform and transparent to obtain the oil composition for cutting the polycrystalline silicon.
In the above technical solution, preferably, when the polycrystalline silicon cutting oil composition contains the odor improver, the odor improver is added after the antioxidant, the lubricating dispersant and the oleic acid are added into the reaction kettle.
In order to solve the third technical problem, the technical scheme adopted by the invention is as follows:
the multipurpose polycrystalline silicon cutting oil composition is applied to the processes of cutting polycrystalline silicon, grinding glass and cutting various metal materials.
The present invention provides a polycrystalline silicon cutting oil composition which exhibits excellent permeability without a surfactant by using a light oil having better penetration spreadability, and thus also has no risk of foaming and corrosion. The introduction of the oily lubricating dispersant with proper molecular weight can balance the effective dispersion of the adhered carborundum in the cutting oil and can just adhere to the glass powder to achieve effective sedimentation，Has the advantages of no need of adding water, convenient use and bodyThe paint has no foaming, good lubricating property, good dispersibility and adhesion, and strong permeability, and can minimize the contact angle of the paint on a Si plate in a short time in a water-based formula ratio; the cutting line cutting device has the advantages that diamond dust can be uniformly and effectively wrapped on the cutting line to keep the sharpness of the cutting line for a long time, a good operation effect can be kept in a low-temperature environment, long-term effective processing efficiency can be kept, the cutting device can be used for processing polycrystalline silicon/optical glass and various metal cutting processing, the universality is strong, and a good technical effect is achieved.
Detailed Description
Example 1:
example 1 discloses a polycrystalline silicon cutting oil composition comprising the following components by mass:
low viscosity base oil: light white oil W1-130 95000g;
high-molecular composite ester: PRIOLUBE 1924000 g
Antioxidant: 2,6-di-tert-butyl-p-cresol 500g;
oleic acid: 500g
Wherein, the macromolecular composite ester PRIOLUBE1929 in this example is produced by Posta.
The preparation method of the polycrystalline silicon cutting oil composition of the embodiment specifically comprises the following steps:
firstly, adding a certain amount of light base oil into a reaction kettle, adding the additive into the reaction kettle according to a proportion, heating to 45 ℃, fully stirring for more than 30min until the mixture is transparent, and finally obtaining the polycrystalline silicon cutting oil composition.
[ example 2 ]
Example 2 discloses a polycrystalline silicon cutting oil composition comprising the following components by mass:
low viscosity base oil: light white oil W1-100 and L-AN 5 total loss system oil (4:6) 96670g;
oxidizing the vegetable oil: oxidized rapeseed oil 2000g
Antioxidant: 500g of octyl/butyl diphenylamine;
oleic acid: 800g;
an odor improver: 30g of ice orange essence;
the preparation method of the polycrystalline silicon cutting oil composition of the present example specifically includes:
firstly, adding a certain amount of light base oil into a reaction kettle, adding the additive into the reaction kettle according to a proportion, and fully stirring at normal temperature for more than 1h until the mixture is transparent, thereby finally obtaining the polycrystalline silicon cutting oil composition.
[ example 3 ]
Example 1 discloses a polycrystalline silicon cutting oil composition comprising the following components by mass:
low viscosity base oil: light white oil W1-130 and L-AN 5 total loss system oil (8:2) 96180g;
polymeric ester: GY-10 3000g
Antioxidant: 2,6-di-tert-butyl-p-cresol 500g;
oleic acid: 300g
An odor improver: 20g of rose essence;
in this example, the polymerized esters GY-10 are manufactured by Lumbo corporation.
The preparation method of the polycrystalline silicon cutting oil composition of the embodiment specifically comprises the following steps:
firstly, adding a certain amount of light base oil into a reaction kettle, adding the additive into the reaction kettle according to a proportion, heating to 45 ℃, fully stirring for more than 30min until the mixture is transparent, and finally obtaining the polycrystalline silicon cutting oil composition.
[ example 4 ]
Example 1 discloses a polycrystalline silicon cutting oil composition comprising the following components by mass:
low viscosity base oil: light white oils W1-130 and W1-100 (7:3) 95980g;
oxidizing the vegetable oil: oxidized rapeseed oil 3000g
Antioxidant: 2,6-di-tert-butyl-p-cresol 500g;
oleic acid: 500g
An odor improver: 20g of ice orange essence;
firstly, adding a certain amount of light base oil into a reaction kettle, adding the additive into the reaction kettle according to a proportion, heating to 45 ℃, fully stirring for more than 30min until the mixture is transparent, and finally obtaining the polycrystalline silicon cutting oil composition.
[ example 5 ]
Example 1 discloses a polycrystalline silicon cutting oil composition comprising the following components by mass:
low viscosity base oil: 1-100 96180g of light white oil W;
polymeric ester: GY-10 3000g
Antioxidant: 2,6-500 g of di-tert-butyl-p-cresol;
oleic acid: 300g
An odor improver: 20g of rose essence;
in this example, the polymerized esters GY-10 are manufactured by Lumbo corporation.
Firstly, adding a certain amount of light base oil into a reaction kettle, adding the additive into the reaction kettle according to a proportion, heating to 45 ℃, fully stirring for more than 30min until the mixture is transparent, and finally obtaining the polycrystalline silicon cutting oil composition.
[ example 6 ]
The polycrystalline silicon wire cutting oil composition of the embodiment 1-5 is applied to diamond dust powder wire cutting polycrystalline silicon blocks, the coating force is strong, the dispersibility is good, no bubbles exist, the cutting efficiency and the qualified product are high, and the single piece processing is completed within 1 hour. The continuous stability is high, and the efficiency can still be kept high under the operation of minus 5 ℃. The corrosion to various metal parts in various machine tool working surfaces and pipeline equipment is avoided.
When large-scale glass is honed, the tool bit feed rate is high, the processing efficiency is high, the glass has no crack, the separation of processing scraps (glass powder) is good, the corrosion and foam tendency is avoided, and daily continuous oil supplement is only needed.
When the grinding tool is used for grinding copper, cast iron, steel and other metals, the metal powder has good settleability, the surface of a machined part has high smoothness and is free from corrosion and discoloration.
[ COMPARATIVE EXAMPLES 1 TO 2 ]
Comparative examples 1 and 2 were prepared according to the respective procedures of example 1, and the component ratios are shown in table 1.
The performance tests of examples 1 to 5 and comparative examples 1 to 2 were carried out, and the obtained performance data are shown in table 2 or table 3 below.
TABLE 1 weight percents of examples 1-5 and comparative examples 1-2
TABLE 2 Performance data of examples 1 to 4 and comparative examples 1 to 2
TABLE 3 Performance data of example 5 and comparative examples 1 to 2
As can be seen from the comparison of the data in the above tables 2 and 3, the oil compositions for polysilicon wire cutting of examples 1 to 5 all meet the requirements of quality standards, have good permeability, no corrosion to various metals, good settleability to glass and metals, good dispersion effect on uniformly dispersed diamond grains in the polysilicon wire cutting, strong processing adaptability of various materials, no bubbling and good low temperature fluidity.
Claims (7)
1. An oil composition for cutting polycrystalline silicon comprises the following components in percentage by weight:
95-97% of low-viscosity base oil,
2-4% of lubricating dispersant,
0.1 to 1 percent of oleic acid,
0.4 to 1 percent of antioxidant;
wherein the low viscosity base oil has a kinematic viscosity at 40 ℃ in the range of 1.5 mm 2 /s~7 mm 2 The low-viscosity base oil is at least one of light white oil, L-AN 5 total loss system oil, isomeric hydrocarbon solvent oil or low-viscosity PAO hydrogenated polydecene; the lubricating dispersant is selected from at least one of oxidized vegetable oil, isomeric vegetable oil, branched polymeric ester or high molecular weight composite ester, and the kinematic viscosity is 35 to 350mm at 100 DEG C 2 S; the antioxidant is at least one of hindered phenol antioxidant or aromatic amine antioxidant.
2. The oil composition for cutting polycrystalline silicon as set forth in claim 1, further comprising, in weight percent: 0.01 to 0.08 percent of odor improver.
3. The oil composition for cutting polycrystalline silicon according to claim 1, wherein the hindered phenol antioxidant is at least one selected from monophenols, alkyl polyphenols and thiobisphenols; the aromatic amine antioxidant is at least one of diarylsecondary amine or p-phenylenediamine.
4. The oil composition for cutting polycrystalline silicon according to claim 2, wherein the odor improver is at least one selected from a citrus aurantium essence or a rose essence.
5. A method for preparing the oil composition for cutting polycrystalline silicon as set forth in claim 1, comprising the steps of: adding the low-viscosity base oil into a blending kettle, uniformly stirring, adding other additives according to the weight percentage, and stirring at normal temperature for 50 to 80min or at 40 to 50 ℃ for 20 to 30min until the mixture is uniform and transparent to obtain the oil composition for cutting the polycrystalline silicon.
6. A method for preparing the oil composition for cutting polycrystalline silicon as set forth in claim 2, comprising the steps of: adding the low-viscosity base oil into a blending kettle, uniformly stirring, adding other additives according to the weight percentage, adding an antioxidant, a lubricating dispersant and oleic acid, and then adding an odor improver; stirring at normal temperature for 50 to 80min or at 40 to 50 ℃ for 20 to 30min until the mixture is uniform and transparent, and obtaining the oil composition for cutting the polycrystalline silicon.
7. Use of the oil composition for cutting polycrystalline silicon according to claim 1 in processes of cutting polycrystalline silicon, grinding glass, and cutting various color metal materials.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10110180A (en) * | 1996-08-12 | 1998-04-28 | Showa Shell Sekiyu Kk | Cutting oil for cut processing with wire saw, cutting oil composition and cutting process of article using the same |
| KR20030088696A (en) * | 2002-05-14 | 2003-11-20 | 한국쉘석유주식회사 | An oil composition for wire sawing process and the cutting method using it |
| CN104357181A (en) * | 2014-09-30 | 2015-02-18 | 宁波保润石化有限公司 | Special magnetic cutting oil and preparation method thereof |
| CN105176647A (en) * | 2015-10-14 | 2015-12-23 | 苏州市晶协高新电子材料有限公司 | Wire-electrode cutting oil and preparation method thereof |
| CN111690456A (en) * | 2020-06-17 | 2020-09-22 | 南京科润工业介质股份有限公司 | Low-volatility lubricating oil applied to trace lubrication process |
-
2020
- 2020-09-29 CN CN202011053821.3A patent/CN112111320B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10110180A (en) * | 1996-08-12 | 1998-04-28 | Showa Shell Sekiyu Kk | Cutting oil for cut processing with wire saw, cutting oil composition and cutting process of article using the same |
| KR20030088696A (en) * | 2002-05-14 | 2003-11-20 | 한국쉘석유주식회사 | An oil composition for wire sawing process and the cutting method using it |
| CN104357181A (en) * | 2014-09-30 | 2015-02-18 | 宁波保润石化有限公司 | Special magnetic cutting oil and preparation method thereof |
| CN105176647A (en) * | 2015-10-14 | 2015-12-23 | 苏州市晶协高新电子材料有限公司 | Wire-electrode cutting oil and preparation method thereof |
| CN111690456A (en) * | 2020-06-17 | 2020-09-22 | 南京科润工业介质股份有限公司 | Low-volatility lubricating oil applied to trace lubrication process |
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