CN102311115A - Preparation method of high-purity green silicon carbide micropowder - Google Patents
Preparation method of high-purity green silicon carbide micropowder Download PDFInfo
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- CN102311115A CN102311115A CN201110245855A CN201110245855A CN102311115A CN 102311115 A CN102311115 A CN 102311115A CN 201110245855 A CN201110245855 A CN 201110245855A CN 201110245855 A CN201110245855 A CN 201110245855A CN 102311115 A CN102311115 A CN 102311115A
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Abstract
The invention relates to a preparation method of a high-purity green silicon carbide micropowder, and is characterized in that the preparation method comprises the following steps of: Step 1, carrying out chemical purification, successively adding green silicon carbide milling, water, sulfuric acid and hydrofluoric acid according to the ratio of 200:180-220:7-10:0.5-2 into a slurry forming pool, fully stirring, reacting for 8-10 hours, removing acid by a centrifuge, placing centrifuged mortar into a rinsing pool for acid bleaching; Step 2, carrying out hydraulic separation by the adoption of a cross-cutting and merging technology, cross-cutting in the later stage of No. 1200 product, merging overflow cylinders with the same rate of progress, carrying out hydraulic separation on a main product No. 1500 again, and carrying out hydraulic separation according to No. 1000-No.800. The preparation method provided by the invention can be used to remove silicate impurities from the raw materials, raise the product purity and increase the yield of main segment number products with the dispersion coefficient of each number being low.
Description
Technical field
The present invention relates to a kind of preparation method who is used for the green silicon carbide powder of silicon wafer cutting, relate in particular to a kind of preparation method of high purity green silicon carbide powder.
Background technology
Green silicon carbide is to be main raw material with refinery coke and high-quality silica, adds salt as scavenging agent, forms through the resistance furnace pyrotic smelting.Its hardness is between corundum and diamond.The greening silicon powder is mainly used in Abrasive Industry, and the high-quality green silicon carbide powder is used for the line cutting of silicon single crystal, polysilicon, arsenic potassium, quartz crystal, is the engineering work material of photovoltaic industry, semiconductor industry, piezoquartz industry.Micro mist class commonly used has: models such as JIS#800, JIS#1000, JIS1200, JSS#1500, JIS#2000, JIS#2500; Satisfy different linear cutting equipments, not collinear cutting material, the personalization in not collinear cutting material diameter, not collinear line of cut footpath requires (the main flow market requirement is #1500, #1200 now).The quality index of green silicon carbide powder mainly comprises purity, size range and concentration degree, foreign matter content, circularity, degree of cleaning, Ph value etc.; Wherein important with silit purity, granularity, circularity, how to improve the difficulty that purity, granularity concentration degree also just become production in process of production.
Existing green silicon carbide powder is the crystolon of smelting in the ore smelting furnace, and its complete processing is: the green silicon carbide piece is smelted--crusher in crushing--Raymond mill abrasive dust--chemical purification--hydraulic classification--operations such as finished product pond sedimentation--fine screen--packing.After pulverizing grinding, can contain Fe, C, a small amount of Al and small amounts of silicate impurity in the green silicon carbide powder raw material of processing, foreign matter content is many in the differential, can reduce the content of silicon in the silit, thereby its hardness is reduced, the cutting effect when influencing follow-up the use.In order to address this problem, existing manufacturer all adopts sulfuric acid that the green silicon carbide powder raw material is carried out pickling, removes Fe and a small amount of Al, goes out C through overflow then, but the small amounts of silicate impurity in the raw material still can not remove, thereby influence final purity.
In addition, existing moisture level is to carry out continuously successively by #2500--#2000--#1500--#1200--#1000--#800, and this each number of series classification mode series products ratio is equity roughly, makes that the concentration degree of product is low, coefficient of dispersion higher (about 28%).This technology has following shortcoming: 1. be unfavorable for tackling turn of the market: the existing market demand is main with #1500, #1200, and this mode major product occupation rate is only less than 60%, and other numbers class sub product ratio is too big, has seriously reduced the core competitiveness of company.2. number class size-grade distribution is wide, coefficient of dispersion is high: owing to be continuous hydraulic classification, lack the granularity reference mark and cause size-grade distribution wide, the probability distribution of size distribution peak value reduces, and has had a strong impact on the cutting efficiency of line cutting.
Summary of the invention
The objective of the invention is to overcome above-mentioned deficiency, provide a kind of and can remove raw material mesosilicic acid salt impurity, improve product purity and improved master's section product yield, the preparation method of the green silicon carbide powder that the coefficient of dispersion of each number is little.
The objective of the invention is to realize like this:
A kind of preparation method of high purity green silicon carbide powder, said method comprises the steps:
Step 1, chemical purification
According to the green silicon carbide abrasive dust: the proportioning of water: sulfuric acid: hydrofluoric acid=200:180-220:7-10:0.5-2, in joining stock tank, proportionally add successively, fully stir; Reaction 8-10h, the whizzer depickling, centrifugal mortar is transferred to rinsing bath and floats acid; Spent acid reclaims to be applied to as mother liquor joins the stock tank use; Unnecessary acid solution is discharged into neutralization tank, adds sheet alkali and quicklime and handles, and is discharged in the environment then;
Step 2, hydraulic classification
Rinsing to neutral green silicon carbide powder is delivered to waterpower overflow cylinder, and adds bubble flower alkali and fully disperse, add the 2# flotation oil then; Remove the C that contains in the green silicon carbide powder raw material; Through carrying out overflow, the flow of control flooding velocity meter is removed the fine powder below the 5 μ m below 300L/ hour then; The flow of control flooding velocity meter carries out the overflow hydraulic classification at 300-1000L/h by the #1800--#1500--#1200 order; Block in the #1200 product later stage, close into water, discharge the upper strata clear water, merge the overflow cylinder of identical progress then, moisture level major product #1500--#1200 again, after press the #1000--#800 classification again.
Said sulfuric acid is with commercially available 98% vitriol oil, and hydrofluoric acid is with commercially available 47% hydrofluoric acid.
The temperature of said water is 50-70 ℃, is good with 60 ℃
Compared with prior art, the invention has the beneficial effects as follows:
The present invention adopts sulfuric acid+hydrofluoric acid fixed proportion pickling impurity removal, effectively removes the impurity such as silicate impurity in the product, can make the raw material about 95% reach the purity more than 99%, exceeds 0.5 percentage point of usual manner.
The spent acid part reclaims as mother liquor and uses, and can reduce production costs, and in addition unnecessary acid solution is carried out comprehensive treating process, non-environmental-pollution.
The present invention adopts hydraulic classification to block merging: be close to turn of the market; The mode that merging is blocked in employing improves the occupation rate of major product (#1500 finished product material and #1200 finished product material); The occupation rate of conventional continuous processing major product accounts for about 65%; Take to block and merge the occupation rate that technology can improve major product and reach 85%, effectively improved the core competitiveness of company.
The coefficient of dispersion of the product that the present invention makes is little; Concentration degree is high: raw material blocks technologies such as merging through chemical purification, waterpower; Effectively improved the size-grade distribution concentration degree of product; Coefficient of dispersion is controlled at below 23%, improves 5 percentage points than usual manner (28%), has effectively improved the cutting efficiency of green silicon carbide powder.
Embodiment
The preparation method of a kind of high purity green silicon carbide powder that the present invention relates to, said method comprises the steps:
Step 1, chemical purification
According to the green silicon carbide abrasive dust: the proportioning of water: sulfuric acid: hydrofluoric acid=200:180-220:7-10:0.5-2, in joining stock tank, proportionally add successively, fully stir; Reaction 8-10h, the whizzer depickling, centrifugal mortar is transferred to rinsing bath and floats acid; Spent acid reclaims to be applied to as mother liquor joins the stock tank use; Unnecessary acid solution is discharged into neutralization tank, adds sheet alkali and quicklime and handles, and is discharged in the environment then;
Said sulfuric acid is with commercially available 98% vitriol oil, and hydrofluoric acid is with commercially available 47% hydrofluoric acid.
The temperature of said water is 50-70 ℃, is the best with 60 ℃.
Step 2, hydraulic classification
Rinsing to neutral green silicon carbide powder is delivered to waterpower overflow cylinder, and adds bubble flower alkali and fully disperse, add the 2# flotation oil then; Remove the C that contains in the green silicon carbide powder raw material, through carrying out overflow, the flow of control flooding velocity meter is below 300L/ hour then; Remove the fine powder below the 5 μ m; After fine powder eliminated, the flow of control flooding velocity meter carried out the overflow hydraulic classification at 300-1000L/h by the #1800--#1500--#1200 order; Block in the #1200 product later stage, close into water, discharge the upper strata clear water, merge the overflow cylinder of identical progress then, moisture level major product #1500--#1200 again, after press the #1000--#800 classification again.
Step 3, aftertreatment
Green silicon carbide powder after the classification is through the sedimentation of finished product pond--fine screen--packaging process makes finished product.
The present invention adopts to block and merges silicon carbide micro-powder and the conventional continuous processing comparing result that technology makes and see the following form:
| ? | Continuous processing | Block merging technology |
| The D of #1500 3 | 5.0 | 5.6 |
| The D of #1500 50 | 8.2-8.7 | 8.4-8.6 |
| The D of #1500 94 | 13.6 | 13.1 |
| The major product occupation rate | 60%--70% | Greater than 85% |
| Coefficient of dispersion | About 28% | Less than 23% |
Claims (5)
1. the preparation method of a high purity green silicon carbide powder, it is characterized in that: said method comprises the steps:
Step 1, chemical purification
According to the green silicon carbide abrasive dust: the proportioning of water: sulfuric acid: hydrofluoric acid=200:180-220:7-10:0.5-2, in joining stock tank, proportionally add successively, fully stir, reaction 8-10h, the whizzer depickling, centrifugal mortar is transferred to rinsing bath and floats acid;
Step 2, hydraulic classification
Rinsing to neutral green silicon carbide powder is delivered to waterpower overflow cylinder, and adds bubble flower alkali and fully disperse, add the 2# flotation oil then; Remove the C that contains in the green silicon carbide powder raw material; Through carrying out overflow, the flow of control flooding velocity meter is removed the fine powder below the 5 μ m below 300L/ hour then; The flow of control flooding velocity meter carries out the overflow hydraulic classification at 300-1000L/h by the #1800--#1500--#1200 order; Block in the #1200 product later stage, close into water, discharge the upper strata clear water, merge the overflow cylinder of identical progress then, moisture level major product #1500--#1200 again, after press the #1000--#800 classification again.
2. the preparation method of a kind of high purity green silicon carbide powder according to claim 1 is characterized in that: said sulfuric acid is with commercially available 98% vitriol oil, and hydrofluoric acid is with commercially available 47% hydrofluoric acid.
3. the preparation method of a kind of high purity green silicon carbide powder according to claim 1 is characterized in that: the temperature of said water is 50-70 ℃.
4. the preparation method of a kind of high purity green silicon carbide powder according to claim 3 is characterized in that: the temperature of said water is 60 ℃.
5. the preparation method of a kind of high purity green silicon carbide powder according to claim 1; It is characterized in that: the spent acid in the said step 1 after the spinning reclaims to be applied to as mother liquor joins the stock tank use; Unnecessary acid solution is discharged into neutralization tank, adds sheet alkali and quicklime and handles.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103028482A (en) * | 2012-12-21 | 2013-04-10 | 无锡晨旸科技股份有限公司 | Alumina micropowder production process |
| CN105668570A (en) * | 2016-01-14 | 2016-06-15 | 宝兴易达光伏刃料有限公司 | Preparation method of silicon wafer cutting edge material |
| CN106744964A (en) * | 2016-11-21 | 2017-05-31 | 西北矿冶研究院 | Process for recovering silicon carbide from silicon carbide waste |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101475172A (en) * | 2008-01-03 | 2009-07-08 | 江源碳化硅微粉有限责任公司 | Recycling, purifying and classifying technology for high purity superfine silicon carbide micro powder |
| JP2009173501A (en) * | 2008-01-28 | 2009-08-06 | Bridgestone Corp | Method of manufacturing high purity silicon carbide powder for silicon carbide single crystal manufacture and silicon carbide single 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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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475172A (en) * | 2008-01-03 | 2009-07-08 | 江源碳化硅微粉有限责任公司 | Recycling, purifying and classifying technology for high purity superfine silicon carbide micro powder |
| JP2009173501A (en) * | 2008-01-28 | 2009-08-06 | Bridgestone Corp | Method of manufacturing high purity silicon carbide powder for silicon carbide single crystal manufacture and silicon carbide single 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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103028482A (en) * | 2012-12-21 | 2013-04-10 | 无锡晨旸科技股份有限公司 | Alumina micropowder production process |
| CN103028482B (en) * | 2012-12-21 | 2014-11-19 | 无锡晨旸科技股份有限公司 | Alumina micropowder production process |
| CN105668570A (en) * | 2016-01-14 | 2016-06-15 | 宝兴易达光伏刃料有限公司 | Preparation method of silicon wafer cutting edge material |
| CN106744964A (en) * | 2016-11-21 | 2017-05-31 | 西北矿冶研究院 | Process for recovering silicon carbide from silicon carbide waste |
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Application publication date: 20120111 |