CN103468346B - Silicon wafer cutting fluid and preparation method thereof - Google Patents

Silicon wafer cutting fluid and preparation method thereof Download PDF

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Publication number
CN103468346B
CN103468346B CN201310412882.8A CN201310412882A CN103468346B CN 103468346 B CN103468346 B CN 103468346B CN 201310412882 A CN201310412882 A CN 201310412882A CN 103468346 B CN103468346 B CN 103468346B
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Prior art keywords
cutting fluid
silicon chip
chip cutting
formamide solution
cutting
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CN103468346A (en
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王欣
周凯鸣
蔺雷亭
刘宏华
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Konca Solar Cell Co Ltd
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Konca Solar Cell Co Ltd
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Abstract

The invention relates to silicon wafer cutting fluid and a preparation method thereof. The silicon wafer cutting fluid mainly comprises PEG (polyethylene glycol), surfactant, lubricant, a penetrant and a chelating agent, as well as formamide solution. The method comprises the steps of adding formamide solution into the silicon wafer cutting fluid, agitating, sealing and storing. A certain proportion of formamide solution is added in the silicon cutting fluid, so that the influence that the pH of the cutting fluid is reduced in storage process can be effectively reduced, the chemical property stability and uniformity of PEG can be guaranteed so as to provide guarantee for the cutting process.

Description

A kind of silicon chip cutting fluid and preparation method thereof
Technical field
The present invention relates to a kind of silicon chip cutting fluid and preparation method thereof.
Background technology
In photovoltaic solar silicon chip cutting process, silicon chip cutting fluid as a kind of auxiliary material consumptive material product that must use in silicon chip cutting process, its consumption along with the silicon chip processing industry of photovoltaic solar industry and China growth and expand.
By by cutting liquid and cutting sand (being generally carborundum) by a certain percentage interworking be mixed to get cutting mortar, and be that carrier drives mortar that silico briquette is cut into silicon chip with cutting steel wire.Multi-wire saw utilizes steel wire side by side to be brought into by cutting mortar in motion process in silico briquette cutting gap, by the barreling effect of abrasive material in mortar, silico briquette is processed into the process of silicon chip.When slicer and human users stable, the stability in the quality of silicon chip processing and cutting process depends primarily on the cutting power of mortar.And pH value is an important parameter of cutting liquid, the size of pH value directly has influence on the service property (quality) of cutting liquid, has great impact to the quality of cutting silicon wafer.
At present, the main component of cutting liquid is polyethylene glycol (PEG), wherein usually can contain a certain proportion of surfactant, lubricant, bleeding agent and intercalating agent etc.The main flow suspension of current multi-wire saw mortar is based on PEG200(polyethylene glycol).Its molecular formula is HOCH 2(CH 2oCH 2) ncH 2oH.In PEG200, n=3, is generally the polymerization of 4 molecules, is formed by ethylene oxide polymerization.
The main performance of PEG has nontoxic, nonirritant, has good water-soluble, and has good intermiscibility with many organic components.There are excellent lubricity, moisture retention, dispersiveness, bonding agent, antistatic additive and softening agent etc. simultaneously.Its lubricity and dispersiveness is mainly applied in multi-wire saw.
The dispersiveness of carborundum in multi-wire saw process in PEG, decides the stability of cutting process and the surface quality of silicon chip.By showing the research of PEG molecular structure and bond energy, strong polar bond makes single PEG be high degree of polarization molecule, the most easily loses the H in-OH in polar bond, combines with the polarity charge carborundum produced because surface coordination is not enough.The isoelectric point of carborundum is near pH=3.9, and the pH value of mortar is when different scopes, and the charge type of silicon carbide is different with charge density, thus makes the saturated extent of adsorption of PEG to carborundum occur difference.
According to measuring and analysis, the pH value of PEG can vary with temperature and change.In PEG molecular structure, the hydrogen that the most active is in hydroxyl.Along with the rising of temperature, interiorly to increase, molecular brownian motion becomes violent, thus is very easy to the hydrogen that loses in hydroxyl, and pH is reduced.
When the SiC distribution of particles in mortar is in PEG, the zeta current potential of its SiC particle depends on pH value, and the unsaturated key mapping of particle surface both can be filled by cation, also can be filled by anion.General in PEG, the isoelectric point of SiC is near pH=3.9.As pH<3.9, the density of particle surface positive charge is greater than negative electrical charge, and zeta current potential is just; As pH>3.9, the negative charge density of particle surface is greater than positive charge, and zeta current potential is negative.
The pH value general control of silicon chip cutting mortar is 5 ~ 8.Within the scope of this, the zeta current potential of SiC particle is negative, and SiC particle surface is filled by negative electrical charge, and whole particle performance is negative electrical charge.Under the electrostatic interaction of negative electrical charge, between SiC particle, form electrostatic repulsion forces.This electrostatic repulsion forces can stop the mutual reunion between SiC particle, thus makes mutually to spread out between SiC particle, prevents mortar from cutting process, agglomeration occurring, avoids having influence on silicon chip cut quality.
In actual production process, find that the pH value of cutting liquid slowly can reduce along with the increase in storage time.After pH is reduced to certain numerical value, significant impact will be produced to chipping qualities.In mortar cutting process, mortar is reunited, and loine pressure is too high, and filter bag blocking can occur, and impact normally cuts production, whole cutter mortar may be caused to scrap, considerably increase production cost time serious.
Therefore, in order to the pH value of cutting liquid can better be controlled, steady production, research finds in cutting liquid, add a certain proportion of pH buffer solvent, the pH value of cutting liquid can be kept within effective life to stablize, the situation that the pH value improving cutting liquid can slowly reduce, thus stop or substantially improve the impact of pH value fluctuation on production and processing quality.
Summary of the invention
The object of the present invention is to provide a kind of silicon chip cutting fluid and preparation method thereof.
Select and add certain organic bases chemical substance in cutting liquid, under the prerequisite not affecting other every physical and chemical performances of cutting liquid, be added into such material a certain amount of, thus make the pH value of cutting liquid keep stable.
For reaching this object, the present invention by the following technical solutions:
The invention provides a kind of silicon chip cutting fluid, described silicon chip cutting fluid, primarily of PEG, surfactant, lubricant, bleeding agent and intercalating agent composition, contains formamide solution in described silicon chip cutting fluid.
The chemical formula of formamide is CH 3nO, is a kind of colourless oil liquid under normal temperature, has alkalescent, hygroscopicity.Its flash-point, burning-point is all higher, and therefore security performance is higher comparatively speaking, and relative density is 1.12, similar with the density of PEG.Its shortcoming has slight excitant and sensitization, therefore needs in actual use to wear chemical protection mirror and rubber gloves.
The present invention adds formamide solution in silicon chip cutting fluid, can increase the resting period of silicon chip cutting fluid, effectively reduces the impact causing the pH value of silicon chip cutting fluid to decline because the resting period is long.
Formamide solution of the present invention accounts for 1 ~ 20wt% of described silicon chip cutting fluid weight, such as, can select 1.02 ~ 19.6wt%, 5 ~ 17.3wt%, 7.2 ~ 14.8wt%, 10 ~ 12.7wt%, 11wt% etc., is preferably 5 ~ 12wt% or is preferably 8 ~ 15wt%.
The concentration of described formamide solution is 99.50%.
Present invention also offers a kind of method preparing silicon chip cutting fluid described above, described method adds described formamide solution in silicon chip cutting fluid, carries out stirring rear hermetically storing.
Described mixing time is 3 ~ 15min, such as, can select 3.01 ~ 14.89min, 4 ~ 12.4min, 5.5 ~ 11min, 8 ~ 10.4min, 9.2min etc., is preferably 5min.
A preparation method for silicon chip cutting fluid, described method specifically comprises the following steps:
1) the silicon chip cutting fluid weight of allocating first is as required to calculate the consumption of required formamide solution;
2) first silicon chip cutting fluid is stirred, in the process stirred, slowly add formamide solution, after waiting solution all to pour into, uniform stirring 5min;
3) deployed silicon chip cutting fluid is canning sealing storage at once, avoids being exposed in air for a long time.
Because present used cutting liquid is all directly filling by production firm, if oneself is modulated, processing cost is higher, may affect to some extent for the cutting liquid quality after processing, and suggestion can by the directly generation processing of the generation manufacturer of cutting liquid.
Before using, by cutting liquid sampling and measuring, pH value keeps stable, in normal range (NR), can normally use.
Compared with prior art scheme, the present invention has following beneficial effect:
In silicon chip cutting fluid, add a certain proportion of formamide solution, effectively can reduce the impact that the pH of cutting liquid in storing process declines, ensure the stable chemical performance of PEG, homogeneous, for cutting process provides safeguard.
Detailed description of the invention
Technical scheme of the present invention is further illustrated below by detailed description of the invention.
For better the present invention being described, be convenient to understand technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows:
Embodiment 1
A kind of silicon chip cutting fluid, its by weight percentage form primarily of following raw material:
Cutting liquid commonly uses raw material 99wt%
Formamide solution 1wt%.
Wherein, the concentration of described formamide solution is 99.50%.
Its preparation method is:
1) the silicon chip cutting fluid weight of allocating first is as required to calculate the consumption of required formamide solution;
2) first silicon chip cutting fluid is stirred, in the process stirred, slowly add formamide solution, uniform stirring 5min after waiting complete soln all to pour into;
3) deployed silicon chip cutting fluid is canning sealing storage at once, avoids being exposed in air for a long time.
Embodiment 2
A kind of silicon chip cutting fluid, its by weight percentage form primarily of following raw material:
Cutting liquid commonly uses raw material 80wt%
Formamide solution 20wt%
Wherein, the concentration of described formamide solution is 99.50%.
Its preparation method is with embodiment 1, and difference is that mixing time is 3min.
Embodiment 3
A kind of silicon chip cutting fluid, its by weight percentage form primarily of following raw material:
Cutting liquid commonly uses raw material 95wt%
Formamide solution 5wt%
Wherein, the concentration of described formamide solution is 99.50%.
Its preparation method is with embodiment 1, and difference is that mixing time is 15min.
Embodiment 4
A kind of silicon chip cutting fluid, its by weight percentage form primarily of following raw material:
Cutting liquid commonly uses raw material 88wt%
Formamide solution 12wt%.
Wherein, the concentration of described formamide solution is 99.50%.
Its preparation method is with embodiment 1, and difference is that mixing time is 10min.
Embodiment 5
A kind of silicon chip cutting fluid, its by weight percentage form primarily of following raw material:
Cutting liquid commonly uses raw material 92wt%
Formamide solution 8wt%
Wherein, the concentration of described formamide solution is 99.50%.
Its preparation method is with embodiment 1, and difference is that mixing time is 5min.
Embodiment 6
A kind of silicon chip cutting fluid, its by weight percentage form primarily of following raw material:
Cutting liquid commonly uses raw material 85wt%
Formamide solution 15wt%
Wherein, the concentration of described formamide solution is 99.50%.
Its preparation method is with embodiment 1, and difference is that mixing time is 8min.
Now by optional one ton of the qualified supplied materials of certain manufacturer's cutting liquid, in this ton of cutting liquid, appoint and get 6 samples (each 1L deposits in sampling bottle), be divided into 2 groups, often organize 3.Wherein 3 samples do not add any solvent, seal up for safekeeping after pH value determination, are labeled as one group, sample.Remain 3 samples, be mixed into formamide solution by consumption of the present invention, after stirring, measure the pH value of these 3 samples, after measurement, 3 samples are sealed up for safekeeping, be labeled as two groups, sample.
Often spend one week to 2 groups of samples and carry out pH value measurement, record related data, table 1 is specific experiment data:
Table 1 specific experiment tables of data
Although can it is evident that the pH value of two groups of samples all slowly declines along with the growth of time by above data, add the pH value of formamide second group of sample, apparently higher than first group of sample.At identical conditions, through the pH of time first group of sample of 5 weeks lower than 6; And the pH of second group is also more than 6, meet use standard.Illustrate at identical conditions, the cutting liquid adding formamide solution than the cutting liquid do not added can the resting period long, thus effectively reduce and make because the resting period is long the pH value of cutting liquid decline to produce adverse influence to silicon chip cutting.
Applicant states, person of ordinary skill in the field is on the basis of above-described embodiment, by the concrete content point value of above-described embodiment component, combined with the technical scheme of summary of the invention part, thus the new number range produced, also be one of record scope of the present invention, the application, for making description simple and clear, no longer enumerates these number ranges.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned detailed description of the invention, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible combination.
In addition, also can be combined between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.

Claims (8)

1. a silicon chip cutting fluid, described silicon chip cutting fluid, primarily of PEG, surfactant, lubricant, bleeding agent and intercalating agent composition, is characterized in that, also containing formamide solution in described silicon chip cutting fluid; Described formamide solution accounts for 1 ~ 20wt% of described silicon chip cutting fluid weight.
2. silicon chip cutting fluid as claimed in claim 1, it is characterized in that, described formamide solution accounts for 5 ~ 12wt% of described silicon chip cutting fluid weight.
3. silicon chip cutting fluid as claimed in claim 1 or 2, it is characterized in that, described formamide solution accounts for 8 ~ 15wt% of described silicon chip cutting fluid weight.
4. silicon chip cutting fluid as claimed in claim 1 or 2, it is characterized in that, the concentration of described formamide solution is 99.50%.
5. prepare a method for silicon chip cutting fluid as described in one of claim 1-4, it is characterized in that, described method adds formamide solution in silicon chip cutting fluid, carries out stirring rear hermetically storing.
6. method as claimed in claim 5, it is characterized in that, described mixing time is 3 ~ 15min.
7. method as claimed in claim 6, it is characterized in that, described mixing time is 5min.
8. the method as described in claim 5 or 6, is characterized in that, said method comprising the steps of:
1) the silicon chip cutting fluid weight of allocating first is as required to calculate the consumption of required formamide solution;
2) first silicon chip cutting fluid is stirred, in the process stirred, slowly add formamide solution, after waiting formamide solution all to pour into, stir 5min;
3) deployed silicon chip cutting fluid is canning sealing storage at once, avoids being exposed in air for a long time.
CN201310412882.8A 2013-09-11 2013-09-11 Silicon wafer cutting fluid and preparation method thereof Active CN103468346B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1858169A (en) * 2006-05-31 2006-11-08 河北工业大学 Semiconductor silicon material water base cutting liquid
CN102851108A (en) * 2012-08-03 2013-01-02 江西赛维Ldk太阳能高科技有限公司 Diamond wire cutting fluid and preparation method thereof
CN103013638A (en) * 2011-09-20 2013-04-03 浙江瑞翌新材料科技有限公司 Water-soluble cooling liquid for fixed abrasive material line cutting, and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1858169A (en) * 2006-05-31 2006-11-08 河北工业大学 Semiconductor silicon material water base cutting liquid
CN103013638A (en) * 2011-09-20 2013-04-03 浙江瑞翌新材料科技有限公司 Water-soluble cooling liquid for fixed abrasive material line cutting, and preparation method thereof
CN102851108A (en) * 2012-08-03 2013-01-02 江西赛维Ldk太阳能高科技有限公司 Diamond wire cutting fluid and preparation method thereof

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