CN104316433A - Analytic method for measuring component content of waste mortar during silicon cutting - Google Patents
Analytic method for measuring component content of waste mortar during silicon cutting Download PDFInfo
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- CN104316433A CN104316433A CN201410652618.6A CN201410652618A CN104316433A CN 104316433 A CN104316433 A CN 104316433A CN 201410652618 A CN201410652618 A CN 201410652618A CN 104316433 A CN104316433 A CN 104316433A
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Abstract
The invention relates to an analytic method for measuring the component content of waste mortar during silicon cutting. The analytic method comprises the following steps: (1) weighing the waste mortar M, drying and weighing the waste mortar M1, and obtaining the moisture content by a constant weight method; (2) adding acetone into the waste mortar obtained in the step (1) according to a mass ratio of 1 to (1-4), soaking, performing centrifugal separation, heating, drying and weighing the waste mortar M2, and obtaining the polyethylene glycol content by the constant weight method; (3) adding diluted hydrochloric acid into the waste mortar obtained in the step (2) according to a mass ratio of 1 to (2-4), soaking, performing centrifugal separation when no bubbles are generated in reaction, flushing solids after reaction by distilled water, heating, drying and weighing the waste mortar M3, and obtaining the metal content by the constant weight method; (4) adding a mixed solution of 48% HF and 30% H2O2 into the waste mortar obtained in the step (3) according to a mass ratio of 1 to (1-1.3), washing with clear water, heating, drying and weighing the waste mortar M4, and obtaining the silicon content by the constant weight method. The method is high in accuracy and precision, easy to perform and relatively low in cost; a measurement method for evaluating the development value of the waste mortar is provided for industry.
Description
Technical field
The present invention relates to a kind of analytical approach measuring silicon cutting waste mortar composition, the method accuracy, precision are high, simple to operate, and cost is lower, for industry provides the one economy of assessment waste mortar Development volue, accurate assay method.
Background technology
In photovoltaic industry and semiconductor manufacturing industry, usually adopt line cutting technology that highly purified monocrystalline silicon and polycrystalline silicon rod are cut into satisfactory silicon chip, in the process, a large amount of waste mortars can be produced.Main containing polyglycol, silicon carbide micro-powder, simple substance silica flour, iron and stainless steel powder etc. in this mortar.If directly discharged by waste mortar, not only to environment, and the serious waste of resource can be caused.Therefore, silicon cutting waste mortar is recycled, there is higher environmental protection and economy and be worth.
It is reported, waste mortar Contents of Main Components (massfraction): 40% ~ 50% polyglycol, 23% ~ 33% carborundum powder, 20% ~ 24% simple substance silica flour, 2.5% ~ 3.0% metal fillings.At present polyglycol, silicon and silit are only limitted to the research of the recycling of waste mortar.Based in production also not accurately and efficiently method component content various in waste mortar is analyzed, cause wastage of material a large amount of in producing, be thus necessary to find the detection method that a kind of economy, accuracy are high.Traditional waste mortar componential analysis technique is more loaded down with trivial details, and accuracy and precision are not high, the shortcoming that consuming cost is high, are unfavorable for the mensuration of the various composition of waste mortar.
Summary of the invention
The object of the invention is to overcome traditional waste mortar component analyzing method and the deficiencies in the prior art, utilize centrifugal separation technology, establish a kind of method of Accurate Measurement waste mortar composition, the method be simple and direct, accuracy and precision high, be suitable for the quantitative test of waste mortar composition.
The invention provides a kind of analytical approach measuring silicon cutting waste mortar composition, it is characterized in that, comprise the following steps:
(1) accurately take waste mortar and be designated as M, by it in 100 ~ 125 DEG C of heating, drying 6 ~ 10h, weigh and be designated as M
1, utilize constant weight method to record moisture in waste mortar;
(2) add acetone in the dry waste mortar obtained to step (1), soak, carry out centrifuging, by the solid heating, drying 4 ~ 7h under 60 ~ 90 DEG C of conditions after centrifugal, note of weighing M
2, utilize constant weight method to record polyethyleneglycol content in waste mortar;
(3) add watery hydrochloric acid in the oven dry waste mortar obtained to step (2), soak, question response bubble-free produces, and carries out centrifuging, and the reacted solid of continuous distilled water flushing, in 100 DEG C ~ 125 DEG C heating, drying 1 ~ 3h, weigh and remember M
3, utilize constant weight method to record tenor in waste mortar;
(4) HF-H is added in the waste mortar obtained to step (3)
2o
2mixed solution, reaction terminate after, with clear water washing, heating, drying 6 ~ 10h under 100 ~ 125 DEG C of conditions, weigh note M
4, utilize constant weight method to record silicone content in waste mortar;
Further, described centrifuging rotating speed is 3000 ~ 7000r/min.
Further, in described step (2), the mass ratio of waste mortar and acetone is 1:1 ~ 4.
Further, in described step (2), waste mortar soaks 5 ~ 8h in acetone, and soaking temperature is 30 ~ 50 DEG C.
Further, in described step (3), the mass ratio of waste mortar and watery hydrochloric acid is 1:2 ~ 4.
Further, in described step (3), with the reacted solid of distilled water flushing 10 ~ 15 times.
Further, in described step (4), mixed solution is by 48%HF and 30%H
2o
2composition.
Further, in described step (4), in mixed solution, 48%HF and 30%H
2o
2mass ratio be 1:1 ~ 1.3.
Beneficial effect of the present invention comprises:
(1) technique is simple, with low cost;
(2) accuracy and precision is high;
(3) measure process cleans environmental protection, meet green requirement of producing.
Accompanying drawing explanation
Technical scheme of the present invention is described in detail referring to accompanying drawing, wherein:
Fig. 1 shows the schematic diagram of the analytical approach measuring silicon cutting waste mortar composition, and operation steps is simple and clear, with low cost, and accuracy and precision is high.
Embodiment
Below in conjunction with specific embodiment and accompanying drawing, the invention will be further described.
The detection technique reported comparatively, under guarantee data accuracy prerequisite, simplifies technique, for industry assessment waste mortar economic worth provides a kind of simple, accurate method.Following (1) ~ (5) of computing formula of the method:
Containing PEG, water and iron filings in the waste mortar reclaimed, according to the feature of its component, the present invention adopts centrifugal separation technology to measure waste mortar composition.
Embodiment one: a kind of analytical approach measuring silicon cutting waste mortar composition, comprises the following steps:
(1) accurately take waste mortar and be designated as M, to put it in air dry oven in 100 DEG C of heating, drying 6h, weigh and be designated as M
1, utilize constant weight method to record moisture in waste mortar;
(2) add acetone in the dry waste mortar obtained to step (1), the mass ratio of waste mortar and acetone is 1:1, under 30 DEG C of conditions, soak 5h, carry out centrifuging, centrifugal rotational speed is 3000r/min, heating, drying 4h under 60 DEG C of conditions, note of weighing M
2, utilize constant weight method to record polyethyleneglycol content in waste mortar;
(3) watery hydrochloric acid is added in the oven dry waste mortar obtained to step (2), the mass ratio of waste mortar and watery hydrochloric acid is 1:2, soak, question response bubble-free produces, carry out centrifuging, centrifugal rotational speed is 3000r/min, and after the reacted solid of continuous distilled water flushing 10 times, in 100 DEG C of heating, drying 1h, note of weighing M
3, utilize constant weight method to record tenor in waste mortar;
(4) 48%HF and 30%H is added in the waste mortar obtained to step (3)
2o
2mixed solution, both mass ratioes are 1:1.1, reaction terminate after, with clear water washing, heating, drying 6h under 100 DEG C of conditions, weigh note M
4, utilize constant weight method to record silicone content in waste mortar;
Embodiment two: a kind of analytical approach measuring silicon cutting waste mortar composition, comprises the following steps:
(1) accurately take waste mortar and be designated as M, to put it in air dry oven in 110 DEG C of heating, drying 8h, weigh and be designated as M
1, utilize constant weight method to record moisture in waste mortar;
(2) add acetone in the dry waste mortar obtained to step (1), the mass ratio of waste mortar and acetone is 1:2, under 40 DEG C of conditions, soak 6h, carry out centrifuging, centrifugal rotational speed is 4000r/min, with heating, drying 5h under 70 DEG C of conditions, and note of weighing M
2, utilize constant weight method to record polyethyleneglycol content in waste mortar;
(3) watery hydrochloric acid is added in the oven dry waste mortar obtained to step (2), the mass ratio of waste mortar and watery hydrochloric acid is 1:3, soak, question response bubble-free produces, carry out centrifuging, centrifugal rotational speed is 4000r/min, and after the reacted solid of continuous distilled water flushing 12 times, in 110 DEG C of heating, drying 2h, note of weighing M
3, utilize constant weight method to record tenor in waste mortar;
(4) 48%HF and 30%H is added in the waste mortar obtained to step (3)
2o
2mixed solution, both mass ratioes are 1:1.2, reaction terminate after, with clear water washing, heating, drying 7h under 110 DEG C of conditions, weigh note M
4, utilize constant weight method to record silicone content in waste mortar;
Embodiment three: a kind of analytical approach measuring silicon cutting waste mortar composition, comprises the following steps:
(1) accurately take waste mortar and be designated as M, to put it in air dry oven in 120 DEG C of heating, drying 9h, weigh and be designated as M
1, utilize constant weight method to record moisture in waste mortar;
(2) add acetone in the dry waste mortar obtained to step (1), the mass ratio of waste mortar and acetone is 1:3, under 40 DEG C of conditions, soak 7h, carry out centrifuging, centrifugal rotational speed is 6000r/min, with heating, drying 6h under 80 DEG C of conditions, and note of weighing M
2, utilize constant weight method to record polyethyleneglycol content in waste mortar;
(3) watery hydrochloric acid is added in the oven dry waste mortar obtained to step (2), the mass ratio of waste mortar and watery hydrochloric acid is 1:3, soak, question response bubble-free produces, carry out centrifuging, centrifugal rotational speed is 6000r/min, and after the reacted solid of continuous distilled water flushing 14 times, in 120 DEG C of heating, drying 2h, note of weighing M
3, utilize constant weight method to record tenor in waste mortar;
(4) 48%HF and 30%H is added in the waste mortar obtained to step (3)
2o
2mixed solution, both mass ratioes are 1:1.2, reaction terminate after, with clear water washing, heating, drying 9h under 120 DEG C of conditions, weigh note M
4, utilize constant weight method to record silicone content in waste mortar;
Embodiment four: a kind of analytical approach measuring silicon cutting waste mortar composition, comprises the following steps:
(1) accurately take waste mortar and be designated as M, to put it in air dry oven in 125 DEG C of heating, drying 10h, weigh and be designated as M
1, utilize constant weight method to record moisture in waste mortar;
(2) add acetone in the dry waste mortar obtained to step (1), the mass ratio of waste mortar and acetone is 1:4, under 50 DEG C of conditions, soak 8h, carry out centrifuging, centrifugal rotational speed is 7000r/min, with heating, drying 7h under 90 DEG C of conditions, and note of weighing M
2, utilize constant weight method to record polyethyleneglycol content in waste mortar;
(3) watery hydrochloric acid is added in the oven dry waste mortar obtained to step (2), the mass ratio of waste mortar and watery hydrochloric acid is 1:4, soak, question response bubble-free produces, carry out centrifuging, centrifugal rotational speed is 7000r/min, and after the reacted solid of continuous distilled water flushing 15 times, in 125 DEG C of heating, drying 3h, note of weighing M
3, utilize constant weight method to record tenor in waste mortar;
(4) 48%HF and 30%H is added in the waste mortar obtained to step (3)
2o
2mixed solution, both mass ratioes are 1:1.3, reaction terminate after, with clear water washing, heating, drying 10h under 125 DEG C of conditions, weigh note M
4, utilize constant weight method to record silicone content in waste mortar;
Obtain waste mortar component content by four examples, its measurement result is as shown in table 1 below.
Table 1 waste mortar composition analysis result
As seen from the above table, this method is easy, can determine impurity content in waste mortar few, and the content of silicon and silit is about 82%, illustrates that waste mortar has higher economic recovery and is worth, is conducive to the recycling of waste mortar.
Although above in conjunction with the embodiments to invention has been detailed description; but; the present invention is not limited to above-mentioned embodiment; in the ken that those of ordinary skill in the art possess; under not departing from the prerequisite of present inventive concept; can also in claims, above-described embodiment is changed or change etc.
Claims (8)
1. measure an analytical approach for silicon cutting waste mortar composition, it is characterized in that, comprise the following steps:
(1) accurately take waste mortar and be designated as M, by it in 100 ~ 125 DEG C of heating, drying 6 ~ 10h, weigh and be designated as M
1, utilize constant weight method to record moisture in waste mortar;
(2) add acetone in the dry waste mortar obtained to step (1), soak, carry out centrifuging, by the solid heating, drying 4 ~ 7h under 60 ~ 90 DEG C of conditions after centrifugal, note of weighing M
2, utilize constant weight method to record polyethyleneglycol content in waste mortar;
(3) add watery hydrochloric acid in the oven dry waste mortar obtained to step (2), soak, question response bubble-free produces, and carries out centrifuging, and the reacted solid of continuous distilled water flushing, in 100 DEG C ~ 125 DEG C heating, drying 1 ~ 3h, weigh and remember M
3, utilize constant weight method to record tenor in waste mortar;
(4) HF-H is added in the waste mortar obtained to step (3)
2o
2mixed solution, reaction terminate after, with clear water washing, heating, drying 6 ~ 10h under 100 ~ 125 DEG C of conditions, weigh note M
4, utilize constant weight method to record silicone content in waste mortar.
2. measure the analytical approach of silicon cutting waste mortar composition as claimed in claim 1, it is characterized in that: described centrifuging rotating speed is 3000 ~ 7000r/min.
3. measure the analytical approach of silicon cutting waste mortar composition as claimed in claim 1, it is characterized in that: in described step (2), the mass ratio of waste mortar and acetone is 1:1 ~ 4.
4. measure the analytical approach of silicon cutting waste mortar composition as claimed in claim 1, it is characterized in that: in described step (2), waste mortar soaks 5 ~ 8h in acetone, and soaking temperature is 30 ~ 50 DEG C.
5. measure the analytical approach of silicon cutting waste mortar composition as claimed in claim 1, it is characterized in that: in described step (3), the mass ratio of waste mortar and watery hydrochloric acid is 1:2 ~ 4.
6. measure the analytical approach of silicon cutting waste mortar composition as claimed in claim 1, it is characterized in that: in described step (3), with the reacted solid of distilled water flushing 10 ~ 15 times.
7. measure the analytical approach of silicon cutting waste mortar composition as claimed in claim 1, it is characterized in that: in described step (4), mixed solution is by 48%HF and 30%H
2o
2composition.
8. measure the analytical approach of silicon cutting waste mortar composition as claimed in claim 1, it is characterized in that: in described step (4), in mixed solution, 48%HF and 30%H
2o
2mass ratio be 1:1 ~ 1.3.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101032806A (en) * | 2006-03-06 | 2007-09-12 | 张捷平 | Method of recycling cutting suspension |
| CN101244823A (en) * | 2008-02-20 | 2008-08-20 | 江南大学 | Method for recycling silicon carbide from by-product in silicon slice cutting process |
| CN101792142A (en) * | 2009-12-31 | 2010-08-04 | 唐康宁 | Method for recovering polysilicon ingots, carborundum powder and polyethylene glycol from cutting waste mortar |
| CN103601191A (en) * | 2013-11-08 | 2014-02-26 | 江南大学 | Method for continuously recycling silicon powder from waste mortar in silicon chip cutting process |
| CN103926165A (en) * | 2014-04-15 | 2014-07-16 | 河南新大新材料股份有限公司 | Detection method for content of solid in silicon wafer cutting mortar |
-
2014
- 2014-11-17 CN CN201410652618.6A patent/CN104316433A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101032806A (en) * | 2006-03-06 | 2007-09-12 | 张捷平 | Method of recycling cutting suspension |
| CN101244823A (en) * | 2008-02-20 | 2008-08-20 | 江南大学 | Method for recycling silicon carbide from by-product in silicon slice cutting process |
| CN101792142A (en) * | 2009-12-31 | 2010-08-04 | 唐康宁 | Method for recovering polysilicon ingots, carborundum powder and polyethylene glycol from cutting waste mortar |
| CN103601191A (en) * | 2013-11-08 | 2014-02-26 | 江南大学 | Method for continuously recycling silicon powder from waste mortar in silicon chip cutting process |
| CN103926165A (en) * | 2014-04-15 | 2014-07-16 | 河南新大新材料股份有限公司 | Detection method for content of solid in silicon wafer cutting mortar |
Non-Patent Citations (1)
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| 王娟等: "硅切割废砂浆制备硅溶胶及回收碳化硅的工艺研究", 《应用化工》 * |
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