CN101979483B - Method for improving dispersibility of silicon carbide mortar - Google Patents
Method for improving dispersibility of silicon carbide mortar Download PDFInfo
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- CN101979483B CN101979483B CN 201010500967 CN201010500967A CN101979483B CN 101979483 B CN101979483 B CN 101979483B CN 201010500967 CN201010500967 CN 201010500967 CN 201010500967 A CN201010500967 A CN 201010500967A CN 101979483 B CN101979483 B CN 101979483B
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Abstract
The invention provides a method for improving the dispersibility of silicon carbide mortar. The method comprises the following steps of: adding a dispersant which is in the mass of 0.001 to 10 percent of that of silicon carbide into 20 to 80 weight percent of a silicon carbide aqueous solution system at the temperature of between 20 and 70 DEG C; stirring for 30 to 120 minutes; after washing with water, controlling the pH of the silicon carbide aqueous solution to be between 3 and 8; and drying to obtain high-dispersibility and high-redispersibility silicon carbide micro powder. The silicon carbide powder processed by the method of the invention is used for cutting monocrystalline silicon and polycrystalline silicon, can effectively shorten the preparation time of cutting fluid mortar, and solves the problem that the silicon carbide micro powder is difficult to redisperse in a cutting or recovering process.
Description
Technical field
The present invention relates to the production of crystalline silicon silicon carbide micro powder for linear cutting or removal process, mention especially dispersibility of silicon carbide mortar is carried out improved a kind of method.
Background technology
In the course of processing of silicon wafer, the sheet material that the linear cutting equipment by special use cuts into different diameter and thickness with silicon rod is present general mode in the world.This cutting process need to use that hardness is high, granularity is little and the silicon carbide of centralized particle diameter as main cutting medium, and add by a certain percentage polyethylene glycol groups or oils is the cutting liquid of main raw material, be used further to cutting after being mixed with mortar.
Silicon carbide deployment conditions of (mortar) in cutting liquid directly affects silicon chip cutting quality and cutting efficiency.At present, the not good counter productive of bringing of mortar dispersiveness is mainly manifested in:
(1) it is longer that mortar is prepared the time, generally more than ten hours.
(2) cohesion between the silicon-carbide particle directly affects the quality that silicon chip cuts, and easily causes the generation of stria and fragment.
(3) silicon-carbide particle is deposited on cutting facility or duct bottom, causes the decline of cutting efficiency.
(4) post-depositional mortar redispersion difficulty gives equipment cleaning and reclaims to process again to make troubles.
At present, for the existing many researchs of the raising of mortar dispersing property, but majority is for the modification of cutting liquid or the adjustment of prescription.And to the introduction of the modification aspect of sand seldom.
Summary of the invention
The present invention is directed to the dispersed and not good defective of redispersibility of existing mortar, provide a kind of silicon carbide micro-powder has been carried out modification, dispersiveness and redispersibility that mortar is used in existing crystalline silicon cutting have been improved, saved mortar setup time, improved quality and the slice efficiency of section, also made things convenient for equipment washing simultaneously and reclaimed again treating processes.
The present invention is by following process implementation:
At 20～70 ℃, it is the dispersion agent that adds silicon carbide quality 0.001～10% in 20～80% the silicon carbide water solution system to weight percent, stir 30～120min, pH with the silicon carbide aqueous solution after washing is controlled at 3～8, and then oven dry namely obtains the silicon carbide micro-powder of polymolecularity and high redispersibility.
Preferred 0.01～5% of the silicon carbide amount of processing of described dispersant dosage.
Described dispersion agent is the following compound of molecular formula:
R
1-(CH
2)
n-R
2
Wherein, n is 0～12 integer; R
1, R
2Can be-OH ,-COOM
1,-SO
3M
2Or-SiO
3M
3, but be not simultaneously-OH; M
1, M
2, M
3Can be hydrogen ion, potassium ion, sodium ion, magnesium ion or ammonium ion.
The preferred sodium octyl of described dispersion agent, sodium oxalate, potassium succinate, oxalic acid, propanedioic acid, hexanodioic acid or hydroxyl magnesium silicate.
The weight percent preferred 30～60% of the silicon carbide in the described silicon carbide aqueous solution.
Described silicon carbide micro-powder can be silicon carbide dry powder, also can be the wet stock in silicon carbide micro-powder production or the removal process.
Described silicon carbide wet stock is the silicon carbide suspension through peracid or alkaline purification, and its pH value is controlled between 4～6.
Preferred 40～60 ℃ of the temperature that described dispersion agent adds;
Preferred 50～the 80min of described churning time.
A kind of preferred method of the present invention can be: at 40～60 ℃, it is the dispersion agent that adds silicon carbide quality 0.01～5% in 30～60% the silicon carbide water solution system to weight percent, stir 50～80min, the pH of the silicon carbide aqueous solution is controlled at 4～6, and then oven dry namely obtains the silicon carbide micro-powder of polymolecularity and high redispersibility.
The mortar that the silicon carbide micro-powder that adopts described method to process is prepared can be used for the silicon chip cutting of monocrystalline or polysilicon.
Method of the present invention can be applied to silicon carbide production or reclaim in the technique, namely increases by a step to the modification of silicon carbide in silicon carbide production or recovery technique.Compared with prior art, its beneficial effect is mainly reflected in following several respects:
1. method of the present invention can make the silicon carbide after the modification be coated with dispersant molecule, can obviously improve dispersing property and the redispersibility of silicon carbide mortar in the less situation of dispersant dosage.
2. method of the present invention is with respect to the method that improves dispersibility of silicon carbide mortar in the prior art by the modification cutting liquid, have simple to operate, many beneficial effects such as implementation is strong.In the prior art, it is dispersed to want to improve mortar by the modification cutting liquid, at first must consider the intermiscibility of dispersion agent and cutting liquid, secondly in the cutting liquid removal process, dispersion agent reclaims difficulty (because the dispersion agent add-on is less, being difficult for reclaiming) on the other hand in cutting liquid and the mortar mixing process, and dispersion agent needs elder generation be adsorbed on equably silicon carbide, play effectiveness, this has just wasted churning time again.And method of the present invention has directly carried out improving the modification of dispersing property to silicon carbide, can very fast silicon carbide be scattered in the cutting liquid, so there are not the problems referred to above.
3. in addition, method of the present invention has improved the dispersiveness of silicon carbide micro-powder in the crystal silicon cutting liquid, has effectively shortened the preparation time of mortar before the cutting; Improve the redispersion performance of silicon carbide mortar, made things convenient for the cleaning of cutting facility and the process that the mortar cyclic regeneration is processed.
Embodiment
Below be specific embodiments of the invention, but method of the present invention and not exclusively being limited, one of ordinary skill in the art can be as required change or omit wherein step.
Used chemical reagent, cutting liquid OX-Si205 (Liaoning AoKe Chemical Co., Ltd's product), 1200# silicon carbide, recovery 1200# silicon carbide, 1500# silicon carbide, recovery 1500# silicon carbide are the commercially available prod in the following instance, and related water is deionized water.
Embodiment one
Silicon carbide micro-powder (1200 with the 500g recovery
#) and 333g water mix and to stir evenly, in the time of 60 ℃, in system, add the 25g sodium octyl, stir 30min, be 5.8 through being washed to silicon carbide aqueous solution pH then, oven dry.Be made in mass ratio mortar A at 1: 1 with cutting liquid OX-Si205, its mortar disperses and the redispersion performance sees Table 1.
Embodiment two
The silicon carbide micro-powder (1500 that 500g is new
#) and 500g water mix and to stir evenly, in the time of 40 ℃, in system, add the 1g sodium oxalate, stir 60min, be 4.8 through being washed to silicon carbide aqueous solution pH then, oven dry.Be made in mass ratio mortar B at 1: 1 with cutting liquid OX-Si205, its mortar disperses and the redispersion performance sees Table 1.
Embodiment three
The silicon carbide micro-powder (1500 that 500g is new
#) and 1166g water mix and to stir evenly, in the time of 50 ℃, in system, add the 5g potassium succinate, stir 80min, be 5.3 through being washed to silicon carbide aqueous solution pH then, oven dry.Be made in mass ratio mortar C at 1: 1 with cutting liquid OX-Si205, its mortar disperses and the redispersion performance sees Table 1.
Embodiment four
Silicon carbide (1200 with the 500g recovery
#) and 500g water mix and to stir evenly, in the time of 40 ℃, in system, add 0.5g oxalic acid, stir 60min, be 4.5 through being washed to silicon carbide aqueous solution pH then, oven dry.Be made in mass ratio mortar D at 1: 1 with cutting liquid OX-Si205, its mortar disperses and the redispersion performance sees Table 1.
Embodiment five
The silicon carbide micro-powder (1500 that 500g is new
#) and 500g water mix and to stir evenly, in the time of 50 ℃, in system, add the 0.5g hydroxyl magnesium silicate, stir 60min, be 4.1 through being washed to silicon carbide aqueous solution pH then, oven dry.Be made in mass ratio mortar E at 1: 1 with cutting liquid OX-Si205, its mortar disperses and the redispersion performance sees Table 1.
Embodiment six
In 1000g waste slurry (sand model 1200
#) in add altogether the 450g deionized water minutes for 3 times, and filter the cutting liquid of removing wherein, get 540g silicon carbide wet material mixture.Add mass concentration in the silicon carbide wet material mixture and be 5% NaOH solution 500g, behind 40 ℃ of stirring reaction 5h, repeatedly being washed to pH value is 6～9, filtration.Add afterwards mass concentration in the silicon carbide mixture after filtration and be 5% HF solution 500g, behind 40 ℃ of stirring reaction 5h, repeatedly being washed to pH value is 3～6, filters to get recovery silicon carbide wet material 450g.In the time of 40 ℃, reclaim adding 400g water and 0.5g hexanodioic acid in the silicon carbide wet material at 450g, stir 60min, be 4.5 through being washed to silicon carbide aqueous solution pH then, oven dry.Be made in mass ratio mortar F at 1: 1 with cutting liquid OX-Si205, its mortar disperses and the redispersion performance sees Table 1.
Comparative Examples
New 1200# silicon carbide and cutting liquid OX-Si205 are made into mortar G in mass ratio at 1: 1;
The 1200# silicon carbide and the cutting liquid OX-Si205 that reclaim are made into mortar H in mass ratio at 1: 1;
New 1500# silicon carbide and cutting liquid OX-Si205 are made into mortar I in mass ratio at 1: 1;
The 1500# silicon carbide and the cutting liquid OX-Si205 that reclaim are made into mortar J in mass ratio at 1: 1.
Dispersiveness and redispersibility evaluation method:
After stirring above-mentioned mortar fully, getting respectively the 100ml mortar volume of packing into is to leave standstill the height of record supernatant liquid in the tool plug graduated cylinder of 100ml under identical temperature humidity condition.Less its suspended dispersed of the height of supernatant liquid is better.
When placing same time, after mortar layer of sand settling height no longer changes, sop up upper strata cutting liquid clear liquid with suction pipe, afterwards graduated cylinder vertically is inverted, be recorded in the identical inversion time (1 hour) the mortar quality that flows out in the graduated cylinder.The mortar quality that flows out is larger, and redispersibility is better.
The dispersiveness of mortar and redispersibility are relatively before and after the modification of table 1. silicon carbide micro-powder
Claims (7)
1. method that improves dispersibility of silicon carbide mortar, may further comprise the steps: at 20 ~ 70 ℃, it is the dispersion agent that adds silicon carbide weight 0.001 ~ 10% in 20 ~ 80% the silicon carbide water solution system to weight percent, stir 30 ~ 120min, the pH of the silicon carbide aqueous solution is controlled at 3 ~ 8, and then oven dry namely obtains the silicon carbide micro-powder of polymolecularity and high redispersibility; Described dispersion agent is sodium octyl, sodium oxalate, potassium succinate, oxalic acid, propanedioic acid, hexanodioic acid or hydroxyl magnesium silicate.
2. method claimed in claim 1, it is characterized in that: described dispersant dosage is 0.01 ~ 5% of pending silicon carbide weight.
3. method claimed in claim 1, it is characterized in that: the weight percent of the silicon carbide in the described silicon carbide aqueous solution is 30 ~ 60%.
4. method claimed in claim 1 is characterized in that: the temperature that described dispersion agent adds is 40 ~ 60 ℃.
5. method claimed in claim 1, it is characterized in that: described churning time is 50 ~ 80min.
6. method claimed in claim 1, it is characterized in that: the pH of the described silicon carbide aqueous solution is controlled at 4 ~ 6.
7. method claimed in claim 1, it is characterized in that: at 40 ~ 60 ℃, it is the dispersion agent that adds silicon carbide quality 0.01 ~ 5% in 30 ~ 60% the silicon carbide water solution system to weight percent, stir 50 ~ 80min, the pH of the silicon carbide aqueous solution is controlled at 4 ~ 6, and then oven dry namely obtains the silicon carbide micro-powder of polymolecularity and high redispersibility.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105462677A (en) * | 2014-09-10 | 2016-04-06 | 新郑市宝德高技术有限公司 | Cutting fluid recovery method |
| CN105084362A (en) * | 2015-07-22 | 2015-11-25 | 河南新大新材料股份有限公司 | Silicon carbide micro-powder siphon grading dispersant for crystal silicon chip cutting and using method of dispersant |
| CN105602522B (en) * | 2015-12-18 | 2018-03-27 | 江西赛维Ldk太阳能高科技有限公司 | A kind of linear cutting mortar and preparation method thereof |
| CN107053507B (en) * | 2017-05-15 | 2019-02-22 | 南通综艺新材料有限公司 | A kind of mortar and its production technology reducing cutting cost |
| CN107523386A (en) * | 2017-07-11 | 2017-12-29 | 青岛远大石墨有限公司 | It is a kind of to be used for cold forging, the lubricant of cold extrusion and preparation method and application method |
| CN110484207B (en) * | 2019-09-20 | 2020-05-29 | 江苏京晶光电科技有限公司 | Preparation method of sapphire wafer fine grinding fluid |
| CN116554953B (en) * | 2023-05-05 | 2024-10-29 | 泰州学院 | Wear-resistant antifriction water-dispersible emulsion for titanium alloy surface and application method thereof |
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|---|---|---|---|---|
| CN101327622A (en) * | 2007-06-21 | 2008-12-24 | 正申科技（北京）有限责任公司 | Mortar recovery technique for cutting single-crystal and polycrystalline silicon wire |
| CN101792141A (en) * | 2010-04-06 | 2010-08-04 | 西安交通大学 | Treatment process of waste mortar in the processing course of silicon crystal |
| CN101804983A (en) * | 2010-04-23 | 2010-08-18 | 连云港佳宇电子材料科技有限公司 | Recovery, purification and classification method of high-purity silicon carbide micro-powder |
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- 2010-10-09 CN CN 201010500967 patent/CN101979483B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101327622A (en) * | 2007-06-21 | 2008-12-24 | 正申科技（北京）有限责任公司 | Mortar recovery technique for cutting single-crystal and polycrystalline silicon wire |
| CN101792141A (en) * | 2010-04-06 | 2010-08-04 | 西安交通大学 | Treatment process of waste mortar in the processing course of silicon crystal |
| CN101804983A (en) * | 2010-04-23 | 2010-08-18 | 连云港佳宇电子材料科技有限公司 | Recovery, purification and classification method of high-purity silicon carbide micro-powder |
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