CN107116708A - A kind of method for analyzing the front and rear silicon-carbide particle change of mortar cutting - Google Patents
A kind of method for analyzing the front and rear silicon-carbide particle change of mortar cutting Download PDFInfo
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- CN107116708A CN107116708A CN201710448298.6A CN201710448298A CN107116708A CN 107116708 A CN107116708 A CN 107116708A CN 201710448298 A CN201710448298 A CN 201710448298A CN 107116708 A CN107116708 A CN 107116708A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28D—WORKING STONE OR STONE-LIKE MATERIALS
- B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
- B28D5/0058—Accessories specially adapted for use with machines for fine working of gems, jewels, crystals, e.g. of semiconductor material
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
The present invention relates to a kind of method for analyzing the front and rear silicon-carbide particle change of mortar cutting, this method includes：Waste mortar after cutting polysilicon is handled, impurity silica flour and iron powder is removed；Then disperse to eliminate agglomeration in dispersant；With the particle diameter and circularity of silicon-carbide particle in mortar before cutting after measurement is scattered, obtained data are compared by the mapping of particle accounting, analysis obtains effective cutting circularity and effective incising control in cutting process.The present invention can be cut for silicon-carbide particle of the different polycrystalline silicon material selections in effective cut coverage, and effective Instructing manufacture makes reasonable, flexible adjustment, improves the utilization rate and cutting efficiency of carborundum, reduce cost.Production, buying simultaneously to fresh sand has certain guidance meaning, by screening, screens, and the stronger batch of selection cutting power can effectively avoid wasting, reduce production cost.With good economic benefit and wide application prospect.
Description
Technical field
The present invention relates to material cutting processing field, and in particular to silicon-carbide particle change before and after one kind analysis mortar cutting
Method.
Background technology
Carborundum is stable due to chemical property, and hardness is high, the advantages of anti-wear performance is good, extensive use and a variety of hard brittle materials
Slice processing process.Existing polysilicon cutting technique is that carborundum and cutting liquid are hybridly prepared into mortar, is carbonized during cutting
Silicon is under the high-speed motion of line of cut, by being rolled to silico briquette, and the mode such as scraping completes cutting.Compared with before cutting, after cutting
Silicon-carbide particle particle diameter is reduced, circularity increase.
In actual cutting process, the distribution situation and cutting power of silicon-carbide particle are closely related.Grain diameter is big, circle
The effect that the low silicon-carbide particle of angle value is cut to polysilicon is bigger, and the particle that particle diameter is small, circularities are high is comparatively to cutting
The effect cut is smaller.Typically it is possible to play the particle diameter of main dissection and the scope of circularity is referred to as effective cut coverage.
In cutting process, if it is possible to the effective cutting circularity and effective incising control of silicon-carbide particle are obtained, with regard to cutting can be derived
During particle abrasion condition, determine the effective range of incising control and circularity.Effectively selected when preparing mortar product
The particle diameter and circularity of silicon-carbide particle, effective guidance can be carried out to production, reasonable, flexible adjustment is made.Simultaneously to new
The production of sand, buying can also carry out certain guidance, and the stronger batch of cutting power is selected in screening, during examination.
Cut polysilicon during, because mortar constantly scrapes silicon rod in cutting process, can drop many silica flours with
And the iron powder of line of cut surface abrasion, these tiny compositions have a strong impact on the judgement to silicon-carbide particle situation in mortar, and
Also damage can be caused to measuring instrument.The complexity for becoming the composition in mortar, the follow-up measurement to silicon-carbide particle of interference, thus
Existing detection mode typically just detects to mortar product, and to the silicon-carbide particle in waste mortar after the completion of cutting simultaneously
Without measurement analysis.
The content of the invention
In view of problems of the prior art, it is an object of the invention to provide be carbonized before and after one kind analysis mortar cutting
The method of silicon grain change.By carrying out removal of impurities processing to the waste mortar after cutting, with carbon in mortar before cutting after measurement removal of impurities
The particle diameter and circularity of silicon carbide particle, obtained data are compared by the mapping of particle accounting, and analysis is obtained effectively cutting circularity and had
Imitate incising control.Effective guidance is carried out to production, the buying of produced on-site and fresh sand using obtained data, cutting is improved
Efficiency, reduces production cost, with good economic benefit and wide application prospect.
For up to this purpose, the present invention uses following technical scheme：
In a first aspect, the present invention provides a kind of method for analyzing the front and rear silicon-carbide particle change of mortar cutting, methods described
Comprise the following steps：
(1) removal of impurities processing is carried out to the waste mortar after cutting polysilicon, concrete operations are：
(a) add alkali lye into the waste mortar after cutting polysilicon to be reacted, separation of solid and liquid after the completion of reaction obtains carbon
Silicon carbide particle；
(b) add acid solution in the silicon-carbide particle obtained to step (a) to be reacted, separation of solid and liquid after the completion of reaction is obtained
Silicon-carbide particle after to removal of impurities；
(2) particle diameter and circularity of silicon-carbide particle in mortar after the removal of impurities that preceding mortar and step (b) are obtained are cut in measurement,
Obtained data are compared by the mapping of particle accounting, analysis obtains effective cutting circularity in cutting process and effectively cuts grain
Footpath.
Mortar of the present invention is the mortar that carborundum and cutting liquid are hybridly prepared into.Polysilicon is cut when with it
Afterwards, the waste mortar after being cut.
The present invention carries out removal of impurities processing to the waste mortar after cutting first, removes impurity silica flour and the iron inside waste mortar
Powder, has obtained pure, soilless sticking silicon-carbide particle, has then measured its particle diameter and circularity, while measuring before cutting in mortar
The particle diameter and circularity of silicon-carbide particle, and obtained data are compared by the mapping of particle accounting.Pass through final test data pair
Than that can obtain cutting the change of front and rear silicon-carbide particle particle diameter and circularity, derive the abrasion condition of particle in cutting process.
Further silicon-carbide particle grain size distribution and circularity variation diagram before and after analysis cutting, obtain effective cutting circle in cutting process
Degree and effective incising control, i.e., effective cut coverage.
Obtain after effective cutting circularity and the effective incising control in cutting process, can select to be in effective cut coverage
Interior silicon-carbide particle is cut to polycrystalline silicon material, and then effective Instructing manufacture, makes reasonable, flexible adjustment.Together
When to the production of fresh sand, purchase also there is certain guidance meaning, pass through screening, screen, the stronger batch of selection cutting power, energy
It is enough effectively to avoid wasting, reduce production cost.
Because the impurity element being mixed into waste mortar is mainly silica flour and iron powder, therefore the present invention first removes silicon using alkali lye
Powder, then removes iron powder, and then obtain the silicon-carbide particle that can measure using acid solution.
According to the present invention, the waste mortar cut after polysilicon is dispersed in water before step (a).
According to the present invention, the volume ratio of the waste mortar and water is 1:(5-20), for example, can be 1:5、1:6、1:7、1:
8、1:9、1:10、1:11、1:12、1:13、1:14、1:15、1:16、1:17、1:18、1:19 or 1:20, and above-mentioned numerical value it
Between specific point value, as space is limited and for concise consideration, it is specific that the present invention no longer scope described in exclusive list includes
Value.The volume ratio of the waste mortar and water is preferably 1:10.
The present invention is to the mode of separation of solid and liquid being related to without particular determination, and the mode of separation of solid and liquid is not constituted
Limitation of the present invention, should be adjusted according to the state of sample and be easy to operation to be advisable.Exemplarily, the separation of solid and liquid
Can be centrifugation, filtering and suction filtration etc., as space is limited and for purposes of brevity, no longer exclusive list.
The purpose that the present invention adds alkali lye is in order to remove the silica flour in the waste mortar after cutting polysilicon, in operating process
Excessive alkali lye should be used, to reach the purpose for removing silica flour completely.
According to the present invention, step (a) alkali lye is sodium hydroxide solution and/or potassium hydroxide solution.
The present invention does not do particular determination to the concentration of alkali lye, as long as the alkali lye added can remove silica flour completely.
According to the present invention, time of step (a) reaction is 0.5-3h, for example can be 0.5h, 1h, 1.5h, 2h,
Specific point value between 2.5h or 3h, and above-mentioned numerical value, as space is limited and for concise consideration, the present invention no longer limit is arranged
Lift the specific point value that the scope includes.The time of step (a) reaction is preferably 1h.
The purpose that the present invention adds acid solution is in order to remove the iron powder in the waste mortar after cutting polysilicon, in operating process
Excessive acid solution should be used, to reach the purpose for removing iron powder completely.
According to the present invention, step (b) acid solution is hydrochloric acid solution.
The present invention does not do particular determination to the concentration of acid solution, as long as the acid solution added can remove iron powder.
According to the present invention, time of step (b) reaction is 1-4h, for example can be 1h, 1.5h, 2h, 2.5h, 3h,
Specific point value between 3.5h or 4h, and above-mentioned numerical value, as space is limited and for concise consideration, the present invention no longer limit is arranged
Lift the specific point value that the scope includes.The time of step (b) reaction is preferably 2h.
According to the present invention, before step (2) is carried out, the silicon-carbide particle after the removal of impurities that step (b) is obtained is dispersed in
In dispersant.
Generally existing agglomeration between due to removing the silicon-carbide particle after impurity element, is unfavorable for follow-up measurement,
Therefore selection is dispersed in dispersant to eliminate agglomeration.
According to the present invention, the dispersant is the combination of P40 and acetone, and the volume ratio of the P40 and acetone are (1-5):
1, for example can be 1:1、1:2、1:3、1:4 or 1:Specific point value between 5, and above-mentioned numerical value, as space is limited and for letter
Bright consideration, the present invention specific point value that no longer scope described in exclusive list includes.The volume ratio of the P40 and acetone is preferably
5:2。
When the combination that dispersant is P40 and acetone, and the volume ratio of the two is 5:When 2, the agglomeration of silicon-carbide particle
It is completely eliminated.
Present invention selection measures the particle diameter of silicon-carbide particle using laser particle analyzer, is measured using Malvern circularity analyzer
The circularity of silicon-carbide particle.Same laser is selected when being measured to the silicon-carbide particle in the mortar before cutting and after cutting
Particle size analyzer and Malvern circularity analyzer, to avoid error.
As preferred technical scheme, a kind of method for analyzing the front and rear silicon-carbide particle change of mortar cutting of the present invention
Comprise the following steps：
(1) removal of impurities processing is carried out to the waste mortar after cutting polysilicon, concrete operations are：
(a) waste mortar cut after polysilicon is dispersed in water, the volume ratio of waste mortar and water is 1:(5-20)；
(b) excessive alkaline reaction 0.5-3h, solid-liquid point are added in the waste mortar and the mixture of water that are obtained to step (a)
From silicon-carbide particle is obtained, the alkali lye is sodium hydroxide solution and/or potassium hydroxide solution；
(c) obtained after excessive hydrochloric acid solution reaction 1-4h, separation of solid and liquid are added in the silicon-carbide particle obtained to step (b)
Silicon-carbide particle after to removal of impurities；
(2) silicon-carbide particle after the removal of impurities for obtaining step (c) is dispersed in dispersant, the dispersant be P40 and
Acetone presses (1-5):The combination of 1 volume ratio；
(3) in the scattered rear mortar that measurement preceding the mortar of cutting and step (2) are obtained respectively the particle diameter of silicon-carbide particle with
Circularity, obtained data are compared by the mapping of particle accounting, and analysis obtains effective cutting circularity in cutting process and effectively cut
Cut particle diameter.
Compared with prior art, the present invention at least has the advantages that：
(1) present invention has obtained effective cutting circularity and the effective incising control in polysilicon cutting process, can be directed to
Silicon-carbide particle of the different polycrystalline silicon material selections in effective cut coverage is cut, and effective Instructing manufacture is done
Go out reasonable, flexible adjustment, improve the utilization rate and cutting efficiency of carborundum, reduce cost.
(2) effective cut coverage of silicon-carbide particle, the life to fresh sand when the present invention can determine cutting polycrystalline silicon material
Production, buying have certain guidance meaning, by screening, screen, the stronger batch of selection cutting power, can be prevented effectively from wave
Take, reduce production cost.
(3) the conventional reagent of present invention selection is handled the mortar after cutting, has obtained pollution-free, soilless sticking phenomenon
Pure silicon-carbide particle, method is simple and easily operated.
Brief description of the drawings
Fig. 1 is the SEM photograph for cutting silicon-carbide particle in the waste mortar after polysilicon；
Fig. 2 is the SEM photograph of the silicon-carbide particle after obtained removal of impurities in the embodiment of the present invention 1；
Fig. 3 is the photo of the silicon-carbide particle handled after removal of impurities in the embodiment of the present invention 1 without dispersant；
Fig. 4 is the photo of the silicon-carbide particle handled after removal of impurities in the embodiment of the present invention 1 by dispersant；
Silicon-carbide particle grain size distribution before and after the cutting that Fig. 5 obtains for the embodiment of the present invention 1 in mortar；
Silicon-carbide particle circularity variation diagram before and after the cutting that Fig. 6 obtains for the embodiment of the present invention 1 in mortar, wherein horizontal sit
Circularity is designated as, ordinate is frequency.
The present invention is described in more detail below.But following examples is only the simple example of the present invention, not generation
Table or limitation the scope of the present invention, protection scope of the present invention are defined by claims.
Embodiment
Further illustrate technical scheme below in conjunction with the accompanying drawings and by embodiment.
For the present invention is better described, technical scheme is readily appreciated, of the invention is typical but non-limiting
Embodiment is as follows：
Embodiment 1
The present embodiment selection is cut the mortar used to polysilicon and measured, and first goes cleavable site to take before measuring
Sample, takes the mortar before same batch cutting and the waste mortar after cutting standby respectively.For the ease of distinguishing, by the mortar before cutting
Mortar product is labeled as, the mortar after cutting is labeled as waste mortar.
The method of silicon-carbide particle change comprises the following steps before and after analysis mortar cutting：
(1) waste mortar after 10ml is cut is dispersed in 100ml deionized waters, uses magnetic stirrer；
(2) sodium hydroxide solution reaction 1h of the 200ml concentration for 1mol/L is added, the rotating speed for then controlling centrifuge is
3500r/min, centrifuges 10min；Silicon-carbide particle is washed with water after the completion of separation, continues to centrifuge, washes, repeat
3 times；
(3) hydrochloric acid solution reaction 2h of the concentration for 1.8mol/L is added, is filtered by vacuum to add water in backward solid and is washed,
Suction filtration after ultrasonically treated 30min, continues to wash, ultrasound, suction filtration is repeated 4 times；
(4) silicon-carbide particle for taking 30mg steps (3) to obtain, adds 10ml water, 5ml P40 and 2ml acetone and is disperseed；
(5) mixture obtained after taking 10ml steps (4) scattered, adds laser particle analyzer and is tested, instrument is shown
Setting is tuned into amounts of particles accounting, tests 30000-33000, obtains silicon-carbide particle particle size interval, utilize Malvern circularity
Analyzer tests equal number of silicon-carbide particle, obtains the distribution proportion of its circularity；
(6) mortar before cutting is dispersed in water rear centrifugal treating, obtains silicon-carbide particle, take carborundum obtained by 30mg
Particle, adds 10ml water, 5ml P40 and 2ml acetone and is disperseed；
(7) mixture obtained after taking 10ml steps (6) scattered, adds laser particle analyzer and is tested, instrument is shown
Setting is tuned into amounts of particles accounting, tests 30000-33000, obtains silicon-carbide particle particle size interval, utilize Malvern circularity
Analyzer tests equal number of silicon-carbide particle, obtains the distribution proportion of its circularity；
(8) data in step (5) and step (7) are compared by the mapping of particle accounting, analysis is obtained in cutting process
Effectively cut circularity and effective incising control.
As shown in Figure 1, the pollutant components such as silica flour and iron powder are mixed with inside waste mortar.As shown in Figure 2, waste mortar is removed
Live together after reason, obtained pure silicon-carbide particle.
From the figure 3, it may be seen that generally existing agglomeration between removing the silicon-carbide particle after impurity.As shown in Figure 4, remove
Silicon-carbide particle after impurity has effectively eliminated agglomeration after dispersant is handled.
As shown in figure 5, silicon-carbide particle grading curve before and after contrast cutting, it can be found that the friendship of cutting anterioposterior curve
Meeting point be all the effective cut coverage of 5.5 microns, i.e. particle diameter be more than 5.5 microns.As shown in fig. 6, before and after contrast cutting
Silicon-carbide particle circularity change curve, finds particle showed increased of the circularity more than 0.930, i.e. silicon-carbide particle after cutting
Circularity, which is maintained at less than 0.930, has preferable cutting power.Therefore, during this batch polysilicon is cut, selection
Particle diameter is more than 5.5 microns, and silicon-carbide particle of the circularity below 0.930 prepares mortar, it is possible to increase cutting efficiency, reduction life
Produce cost；When production in fresh sand, buying, the product of above-mentioned effective cut coverage is selected as far as possible, wastes can be prevented effectively from, drop
Low production cost.
The preferred embodiment of the present invention described in detail above, still, the present invention are not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (10)
1. a kind of method for analyzing the front and rear silicon-carbide particle change of mortar cutting, it is characterised in that methods described includes following step
Suddenly：
(1) removal of impurities processing is carried out to the waste mortar after cutting polysilicon, concrete operations are：
(a) add alkali lye into the waste mortar after cutting polysilicon to be reacted, separation of solid and liquid after the completion of reaction obtains carborundum
Particle；
(b) add acid solution in the silicon-carbide particle obtained to step (a) to be reacted, separation of solid and liquid after the completion of reaction is removed
Silicon-carbide particle after miscellaneous；
(2) particle diameter and circularity of silicon-carbide particle in mortar after the removal of impurities that preceding mortar and step (b) are obtained are cut in measurement, will
To data compare by the mapping of particle accounting, analysis obtains effective cutting circularity and effective incising control in cutting process.
2. the method as described in claim 1, it is characterised in that the waste mortar point after polysilicon will be cut before step (a)
It is dispersed in water；
Preferably, the volume ratio of the waste mortar and water is 1:(5-20), preferably 1:10.
3. method as claimed in claim 1 or 2, it is characterised in that step (a) alkali lye be sodium hydroxide solution and/or
Potassium hydroxide solution；
Preferably, excessive alkali lye is added in step (a).
4. the method as described in claim any one of 1-3, it is characterised in that the time of step (a) reaction is 0.5-3h,
Preferably 1h.
5. the method as described in claim any one of 1-4, it is characterised in that step (b) acid solution is hydrochloric acid solution；
Preferably, excessive acid solution is added in step (b).
6. the method as described in claim any one of 1-5, it is characterised in that the time of step (b) reaction is 1-4h, excellent
Elect 2h as.
7. the method as described in claim any one of 1-6, it is characterised in that before step (2) is carried out, step (b) is obtained
To removal of impurities after silicon-carbide particle be dispersed in dispersant.
8. method as claimed in claim 7, it is characterised in that the dispersant is the combination of P40 and acetone；
Preferably, the volume ratio of the P40 and acetone are (1-5):1, preferably 5:2.
9. the method as described in claim any one of 1-8, it is characterised in that measure carbon using laser particle analyzer in step (2)
The particle diameter of silicon carbide particle, the circularity of silicon-carbide particle is measured using Malvern circularity analyzer.
10. the method as described in claim any one of 1-9, it is characterised in that the described method comprises the following steps：
(1) removal of impurities processing is carried out to the waste mortar after cutting polysilicon, concrete operations are：
(a) waste mortar cut after polysilicon is dispersed in water, the volume ratio of waste mortar and water is 1:(5-20)；
(b) excessive alkaline reaction 0.5-3h is added in the waste mortar and the mixture of water that are obtained to step (a), separation of solid and liquid is obtained
To silicon-carbide particle, the alkali lye is sodium hydroxide solution and/or potassium hydroxide solution；
(c) removed after excessive hydrochloric acid solution reaction 1-4h, separation of solid and liquid are added in the silicon-carbide particle obtained to step (b)
Silicon-carbide particle after miscellaneous；
(2) silicon-carbide particle after the removal of impurities for obtaining step (c) is dispersed in dispersant, and the dispersant is P40 and acetone
By (1-5):The combination of 1 volume ratio；
(3) particle diameter and circularity of silicon-carbide particle in the scattered rear mortar that preceding mortar and step (2) are obtained are cut in measurement respectively,
Obtained data are compared by the mapping of particle accounting, analysis obtains effective cutting circularity in cutting process and effectively cuts grain
Footpath.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710448298.6A CN107116708B (en) | 2017-06-14 | 2017-06-14 | A method of analysis mortar cutting front and back silicon-carbide particle variation |
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| CN201710448298.6A CN107116708B (en) | 2017-06-14 | 2017-06-14 | A method of analysis mortar cutting front and back silicon-carbide particle variation |
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| CN108099035A (en) * | 2017-12-21 | 2018-06-01 | 重庆超硅半导体有限公司 | A kind of integrated circuit monocrystalline silicon multi-wire saw stability control method |
| CN110702490A (en) * | 2019-11-01 | 2020-01-17 | 上海申和热磁电子有限公司 | Method for purifying and analyzing silicon carbide in semiconductor slice waste liquid |
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| CN110702490A (en) * | 2019-11-01 | 2020-01-17 | 上海申和热磁电子有限公司 | Method for purifying and analyzing silicon carbide in semiconductor slice waste liquid |
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|---|---|
| CN107116708B (en) | 2019-05-28 |
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