CN113310903A - Method for measuring content of micro silicon powder in polycrystalline silicon material - Google Patents
Method for measuring content of micro silicon powder in polycrystalline silicon material Download PDFInfo
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- CN113310903A CN113310903A CN202110583682.3A CN202110583682A CN113310903A CN 113310903 A CN113310903 A CN 113310903A CN 202110583682 A CN202110583682 A CN 202110583682A CN 113310903 A CN113310903 A CN 113310903A
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Abstract
The invention relates to a method for measuring the content of micro silicon powder in a polycrystalline silicon material. A method for measuring the content of micro silicon powder in a polycrystalline silicon material comprises the following steps: (1) completely soaking the polycrystalline silicon material in water to enable micro silicon powder in the polycrystalline silicon material to enter the water, and then removing the polycrystalline silicon material to obtain a solution 1; (2) the content of the microsilica in the solution 1 was measured by the turbidity method. The method for measuring the content of the micro silicon powder in the polycrystalline silicon material is simple and can more accurately measure the content of the micro silicon powder in the polycrystalline silicon material.
Description
Technical Field
The invention belongs to the technical field of polycrystalline silicon, and particularly relates to a method for measuring the content of micro silicon powder in a polycrystalline silicon material.
Background
The polysilicon materials can be mutually extruded and rubbed in the processes of crushing, packaging and conveying, so that certain micro silicon powder can be generated on the surface of the silicon block. And the pollution impurities of the polysilicon material in the air, the pollution impurities generated in the contact process with auxiliary materials and the like and the pollution impurities generated in the crushing process of the silicon material are all present in the micro silicon powder. Therefore, the removal of the microsilica in the polysilicon material is equivalent to the removal of the contaminating impurities in the polysilicon material.
At present, the silicon material is produced in the industry by adopting a screening mode, and the micro silicon powder is also removed by adopting the screening mode. However, the micro silicon powder cannot be completely removed by the screening method, so that the crystallization rate and the minority carrier lifetime of the single crystal pulling in the downstream process are affected.
Due to the influence of the micro silicon powder on the quality of downstream products, the determination of the content of the micro silicon powder in the polycrystalline silicon material is important before the polycrystalline silicon material is used in the early stage. The content of the micro silicon powder on the surface of the silicon block is mainly measured by a quantitative method after screening, but the screening capacity is limited, and the micro silicon powder cannot be completely screened out, so that the measurement accuracy is poor.
In view of this, the invention provides a novel method for measuring the content of the micro silicon powder in the polycrystalline silicon material, which can more accurately measure the content of the micro silicon powder in the polycrystalline silicon material.
Disclosure of Invention
The invention aims to provide a method for measuring the content of micro silicon powder in a polycrystalline silicon material, which is simple to operate and can effectively measure the content of the micro silicon powder in the polycrystalline silicon material.
In order to realize the purpose, the adopted technical scheme is as follows:
a method for measuring the content of micro silicon powder in a polycrystalline silicon material comprises the following steps:
(1) completely soaking the polycrystalline silicon material in water to enable micro silicon powder in the polycrystalline silicon material to enter the water, and then removing the polycrystalline silicon material to obtain a solution 1;
(2) the content of the microsilica in the solution 1 was measured by the turbidity method.
Further, in the step (1), the soaking time is 10-15 min.
Still further, in the step (1), the soaking time is 10 min.
Further, in the step (1), the water surface is 3-5cm higher than the polysilicon material.
Further, in the step (1), the water is ultrapure water.
Further, in the step (2), before the turbidity method detection, the solution 1 is stirred to uniformly distribute the micro silicon powder in the solution 1.
Further, in the step (2), when the turbidity method detection is performed, the detection is repeated at least 3 times, and the average value of the results is taken as the final result.
Compared with the prior art, the invention has the beneficial effects that:
1. the method for measuring the content of the micro silicon powder in the polycrystalline silicon material is simple to operate, the amount of the micro silicon powder in each package of the silicon material is transversely evaluated by a turbidity method, and the content of the micro silicon powder in the polycrystalline silicon material can be effectively measured, so that the amount of the silicon powder in the silicon material can be controlled in the production process, the content of metal impurities on the surface of the silicon material is reduced, and the crystallization rate and the minority carrier lifetime of single crystal pulling in a downstream process are improved.
2. The method for measuring the content of the micro silicon powder in the polycrystalline silicon material can monitor the process stability in the processing process of the silicon material through the change of turbidity. If the turbidity changes greatly, the processing process has problems and can be adjusted in time.
3. According to the method for measuring the content of the micro silicon powder in the polycrystalline silicon material, the subsequent use of the polycrystalline silicon material is not influenced after the measurement.
Drawings
FIG. 1 is a graph showing a change in a turbidity detection value when a water amount is fixed;
FIG. 2 is a graph showing the change of turbidity detection values with fixed soaking time.
Detailed Description
In order to further illustrate the method for measuring the content of microsilica in a polysilicon material according to the present invention to achieve the intended purpose of the invention, the following embodiments, structures, features and effects thereof will be described in detail. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The method for measuring the content of the microsilica in the polysilicon material according to the present invention will be further described in detail with reference to the following specific examples:
at present, the detection of the micro silicon powder in the silicon material adopts a method of weighing after screening, namely screening the micro silicon powder in the silicon material by using sieves with different apertures, and weighing the weight of the micro silicon powder. However, this method has the following disadvantages: 1) the method is easy to pollute the silicon material; 2) because the micro silicon powder has small particle size, the micro silicon powder cannot be effectively screened out through a sieve. Therefore, the existing screening and weighing method can only indirectly reflect the content of the micro silicon powder in the silicon material, cannot accurately express the actual content of the micro silicon powder in each package of the silicon material, and particularly cannot separate the micro silicon powder in the gap of the silicon material in a screening mode. The content of the micro silicon powder in the invention can not be corresponded by the existing screening and weighing mode.
The technical scheme of the invention is as follows:
a method for measuring the content of micro silicon powder in a polycrystalline silicon material comprises the following steps:
(1) completely soaking the polycrystalline silicon material in water to enable micro silicon powder in the polycrystalline silicon material to enter the water, and then removing the polycrystalline silicon material to obtain a solution 1;
(2) the content of the microsilica in the solution 1 was measured by the turbidity method.
Further, in the step (1), the soaking time is 10-15 min.
Still further, in the step (1), the soaking time is 10 min.
Further, in the step (1), the water surface is 3-5cm higher than the polysilicon material.
Further, in the step (1), the water is ultrapure water. By adopting ultrapure water, the micro silicon powder can be better introduced into water.
All tests must be performed under the same conditions for contrast, and the amount of water is selected according to the volume of the container used.
Further, in the step (2), before the turbidity method detection is performed, the solution 1 is stirred, so that the micro silicon powder in the solution 1 is uniformly distributed, and the detection accuracy is more favorable.
Further, in the step (2), when the turbidity method detection is performed, the detection is repeated at least 3 times, and the average value of the results is taken as the final result.
Example 1.
The specific operation steps are as follows:
(1) sampling is carried out on each packet of 10kg of polycrystalline silicon material according to the minimum packaging specification produced in the polycrystalline silicon industry.
(2) The whole package of silicon material was poured into a 35L plastic box which was cleaned in advance.
(3) And slowly adding 12L of ultrapure water to flush the micro silicon powder on the surface of the polycrystalline silicon material, so that the polycrystalline silicon material is completely submerged below the horizontal plane.
(4) And then soaking for 6, 8, 10, 12 and 15 minutes respectively to enable the micro silicon powder in the polycrystalline silicon material to enter the ultrapure water.
(5) Then pouring the solution into another clean 35L plastic box, simultaneously filtering out polysilicon materials, and uniformly stirring the solution by using a clean glass rod to uniformly distribute the silicon micropowder in the solution to obtain a solution 1.
(6) A sample was taken from the solution 1 and placed in a turbidity test specimen bottle (10 ml).
(7) Then the sample bottle is put into a sample pool of a turbidity detector which is calibrated in advance for detection, the turbidity data is read and recorded, and 3 groups of data are repeatedly detected in this way, and the average value is taken.
The polycrystalline silicon material is coral single crystal small material (linear size 8-50mm, 10 kg/bag), and the detection data is shown in table 1.
TABLE 1
Based on the data in Table 1, a graph of FIG. 1, which shows the change in the turbidity detected with the amount of added water, is plotted.
The volume of the container used in this embodiment is about 35L of a cuboid transparent plastic box, and in order to ensure that all silicon materials are completely soaked below the water surface, and the water surface is higher than the silicon material plane by about 3-5cm, so as to achieve the purpose of facilitating observation of the phenomenon in the whole process, 12L of water is selected for the silicon materials soaked in 10kg of water.
As can be seen from fig. 1 and table 1, the optimum soaking time was 10 minutes. Because the turbidity of the solution was substantially stable after 10 minutes with little relative change.
Example 2.
The specific operation steps are as follows:
(1) sampling is carried out on each packet of 10kg of polycrystalline silicon material according to the minimum packaging specification produced in the polycrystalline silicon industry.
(2) The whole package of silicon material was poured into a 35L plastic box which was cleaned in advance.
(3) 13L of ultrapure water is slowly added to wash the micro silicon powder on the surface of the polycrystalline silicon material, so that the polycrystalline silicon material is completely submerged below the horizontal plane.
(4) And soaking for 10 minutes to enable the micro silicon powder in the polycrystalline silicon material to enter the ultrapure water.
(5) Then pouring the solution into another clean 35L plastic box, simultaneously filtering out polysilicon materials, and uniformly stirring the solution by using a clean glass rod to uniformly distribute the silicon micropowder in the solution to obtain a solution 1.
(6) A sample was taken from the solution 1 and placed in a turbidity test specimen bottle (10 ml).
(7) Then the sample bottle is put into a sample pool of a turbidity detector which is calibrated in advance for detection, the turbidity data is read and recorded, and 3 groups of data are repeatedly detected in this way, and the average value is taken.
Example 3.
The specific procedure of example 3 is the same as that of example 2, except that 14L of ultrapure water is added in step (3) to rinse the microsilica on the surface of the polysilicon mass, so that the polysilicon mass is completely submerged below the water level.
Example 4.
The specific procedure of example 4 is the same as that of example 2, except that 15L of ultrapure water is slowly added in step (3) to rinse the microsilica on the surface of the polysilicon mass, so that the polysilicon mass is completely submerged below the water level.
Example 5.
The specific procedure of example 3 is the same as that of example 2, except that 16L of ultrapure water is slowly added in step (3) to rinse the microsilica on the surface of the polysilicon mass, so that the polysilicon mass is completely submerged below the water level.
The polysilicon material used in examples 2-5 was small coral single crystal material (linear size 8-50mm, 10 kg/package) and the test data are shown in Table 2.
TABLE 2
Based on the data in Table 2, a graph 2 showing the change in the turbidity detection value with the fixed soaking time is plotted.
As can be seen from Table 2 and FIG. 2, the selection of the amount of water has a certain relationship with the volume of the vessel used, and the more the amount of water used, the smaller the turbidity value measured for the same weight of silicon material. Therefore, the invention selects the water consumption according to the principle that the silicon material is completely submerged in water, and finally selects the water consumption of 12L.
The method for measuring the content of the micro silicon powder in the polycrystalline silicon material is simple to operate, the amount of the micro silicon powder in each package of the silicon material is transversely evaluated by a turbidity method, and the content of the micro silicon powder in the polycrystalline silicon material can be effectively measured, so that the amount of the silicon powder in the silicon material can be adjusted in the production process, the content of metal impurities on the surface of the silicon material is reduced, and the crystallization rate and the minority carrier lifetime of single crystal pulling in a downstream process are improved. And the subsequent use of the polysilicon material is not influenced after the determination.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (7)
1. A method for measuring the content of micro silicon powder in a polycrystalline silicon material is characterized by comprising the following steps:
(1) completely soaking the polycrystalline silicon material in water to enable micro silicon powder in the polycrystalline silicon material to enter the water, and then removing the polycrystalline silicon material to obtain a solution 1;
(2) the content of the microsilica in the solution 1 was measured by the turbidity method.
2. The method of measuring according to claim 1,
in the step (1), the soaking time is 10-15 min.
3. The method of measuring according to claim 2,
in the step (1), the soaking time is 10 min.
4. The method of measuring according to claim 1,
in the step (1), the water surface is 3-5cm higher than the polysilicon material.
5. The method of measuring according to claim 1,
in the step (1), the water is ultrapure water.
6. The method of measuring according to claim 1,
in the step (2), before the turbidity method detection, the solution 1 is stirred to uniformly distribute the micro silicon powder in the solution 1.
7. The method of measuring according to claim 1,
in the step (2), when the turbidity method detection is carried out, the detection is repeated at least 3 times, and the average value of the results is taken as the final result.
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Citations (5)
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| JP2012062206A (en) * | 2010-09-14 | 2012-03-29 | Mitsubishi Materials Corp | Classifier and sorter of polycrystalline silicon |
| CN102502652A (en) * | 2011-11-07 | 2012-06-20 | 江西旭阳雷迪高科技股份有限公司 | Cleaning process for polycrystalline material |
| CN107676088A (en) * | 2016-08-02 | 2018-02-09 | 中国石油天然气股份有限公司 | Method for monitoring content of coal dust in coal-bed gas well output liquid |
| CN111198116A (en) * | 2018-11-20 | 2020-05-26 | 宁波江丰电子材料股份有限公司 | Target detection method |
| WO2021034937A1 (en) * | 2019-08-19 | 2021-02-25 | Boortz Christopher Lee | Particulate matter detection device |
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- 2021-05-27 CN CN202110583682.3A patent/CN113310903A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012062206A (en) * | 2010-09-14 | 2012-03-29 | Mitsubishi Materials Corp | Classifier and sorter of polycrystalline silicon |
| CN102502652A (en) * | 2011-11-07 | 2012-06-20 | 江西旭阳雷迪高科技股份有限公司 | Cleaning process for polycrystalline material |
| CN107676088A (en) * | 2016-08-02 | 2018-02-09 | 中国石油天然气股份有限公司 | Method for monitoring content of coal dust in coal-bed gas well output liquid |
| CN111198116A (en) * | 2018-11-20 | 2020-05-26 | 宁波江丰电子材料股份有限公司 | Target detection method |
| WO2021034937A1 (en) * | 2019-08-19 | 2021-02-25 | Boortz Christopher Lee | Particulate matter detection device |
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Application publication date: 20210827 |