CN111017929B - Silicon material cleaning method - Google Patents
Silicon material cleaning method Download PDFInfo
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- CN111017929B CN111017929B CN201911366795.7A CN201911366795A CN111017929B CN 111017929 B CN111017929 B CN 111017929B CN 201911366795 A CN201911366795 A CN 201911366795A CN 111017929 B CN111017929 B CN 111017929B
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/037—Purification
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Abstract
The invention discloses a silicon material cleaning method, which comprises the following steps: (1) adding liquid caustic soda into the silicon material, and stirring for 3-5 min; (2) sieving with a coarse sieve to obtain a first alkali washing silicon material and a first alkali residual liquid, and sieving with a fine sieve to obtain a second alkali residual liquid; (3) adding the second alkaline residual liquid into the first alkaline silicon washing material, heating to 30 ℃, and performing first ultrasonic cleaning; (4) adding sodium sulfate into the second alkali residual liquid, heating to 80-90 ℃, and continuously performing second ultrasonic cleaning in the heating process; (5) and continuously injecting water into the second alkali residual liquid, and simultaneously discharging liquid, and continuously performing third ultrasonic cleaning in the process to obtain a second alkali silicon cleaning material. According to the invention, alkali liquor is matched with sodium sulfate, ultrasonic cleaning is carried out for multiple times, and water injection and drainage are carried out while the third ultrasonic cleaning is carried out, so that the cleaning effect is improved; the alkali liquor is recycled, so that the use amount of the alkali liquor is reduced, and the cleaning cost is saved.
Description
Technical Field
The invention relates to the technical field of silicon material processing, in particular to a silicon material cleaning method.
Background
In the photovoltaic industry or in the field of semiconductor technology, there is a need to produce silicon wafers from the slicing process of silicon stock.
The silicon material must be cleaned, including acid and alkali cleaning, before use. The alkali washing is generally to soak the silicon material in alkali liquor, and then perform ultrasonic cleaning, and may also adopt manual stirring, so as to accelerate the removal of impurities on the surface of the silicon material.
In the existing alkali washing process, single soaking and washing are adopted, the washing effect is poor, and therefore more alkali liquor is needed to be used to meet the washing requirement.
Disclosure of Invention
The invention aims to provide a silicon material cleaning method with a good cleaning effect.
A silicon material cleaning method comprises the following steps:
(1) adding liquid caustic soda into the silicon material, and stirring for 3-5 min;
(2) sieving with a coarse sieve to obtain a first alkali washing silicon material and a first alkali residual liquid, and sieving with a fine sieve to obtain a second alkali residual liquid;
(3) adding the second alkaline residual liquid into the first alkaline silicon washing material, heating to 30 ℃, and performing first ultrasonic cleaning;
(4) adding sodium sulfate into the second alkali residual liquid, heating to 80-90 ℃, and continuously performing second ultrasonic cleaning in the heating process;
(5) and continuously injecting water into the second alkali residual liquid, and simultaneously discharging liquid, and continuously performing third ultrasonic cleaning in the process to obtain a second alkali silicon cleaning material.
The invention has the beneficial effects that: the alkali liquor is matched with the sodium sulfate, multiple times of ultrasonic cleaning are performed, and water injection and drainage are performed while the third ultrasonic cleaning is performed, so that the cleaning effect is improved; the alkali liquor is recycled, so that the use amount of the alkali liquor is reduced, and the cleaning cost is saved.
In addition, the silicon material cleaning method provided by the invention can also have the following additional technical characteristics:
further, the alkali liquor in the step (1) is sodium hydroxide, potassium hydroxide or sodium methoxide.
Further, the concentration of the alkali liquor in the step (1) is 3-10 mol/L.
Further, the coarse mesh sieve in the step (2) is 20-100 meshes, and the fine mesh sieve is 150-200 meshes.
Further, the heating temperature rise range in the step (4) is 0.5-2 ℃/min.
Further, the temperature rise process of the heating in the step (4) is as follows:
raising the temperature to 50 ℃ with the temperature rise amplitude of 1 ℃/min;
raising the temperature to 70 ℃ with the temperature rise amplitude of 0.5 ℃/min;
raising the temperature to 80-90 ℃ at a temperature rise of 2 ℃/min.
Further, the concentration of the sodium sulfate in the step (4) is 1-5 mol/L.
Further, the water injection speed of the injected water in the step (5) is equal to the liquid outlet speed of the discharged liquid.
Further, the water injection speed of the injected water in the step (5) is 1.2-1.5 times of the liquid outlet speed of the discharged liquid.
Further, the duration time of the third ultrasonic cleaning in the step (5) is 10-20 min.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
In order to make the objects, features and advantages of the present invention comprehensible, specific embodiments accompanied with examples are described in detail below. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Example 1
A silicon material cleaning method comprises the following steps:
(1) adding liquid alkali into the silicon material, and stirring for 3min, wherein the liquid alkali is sodium hydroxide, and the concentration is 3 mol/L;
(2) sieving with a coarse sieve to obtain a first alkali washing silicon material and a first alkali residual liquid, and sieving with a fine sieve to obtain a second alkali residual liquid;
(3) adding the second alkaline residual liquid into the first alkaline silicon washing material, heating to 30 ℃, and performing first ultrasonic cleaning;
(4) adding sodium sulfate into the second alkali residual liquid, heating to 80 ℃ with the concentration of the sodium sulfate being 1mol/L, wherein the temperature rise range is 0.5 ℃/min, and continuously performing second ultrasonic cleaning in the heating process;
(5) and continuously injecting water into the second alkaline residual liquid, and simultaneously discharging the liquid, wherein the water injection speed v1 of the injected water is equal to the liquid outlet speed v2 of the discharged liquid, namely v1 is equal to v2, and the third ultrasonic cleaning is continuously performed in the process for 10min to obtain a second alkaline silicon washing material.
The second alkali-washed silica material is the final product after washing in this example.
In this embodiment, the volume of the second alkaline raffinate is V0, V1 is 0.2V0/min, and the process continues to perform the third ultrasonic cleaning, for example, V0 is 100L, and V1 is 20L/min.
It is understood that the present embodiment uses liquid caustic soda, and those skilled in the art can know that the effect of the present embodiment can be achieved by using a mixed liquid of caustic soda flakes and water.
It should be noted that the first ultrasonic cleaning, the second ultrasonic cleaning and the third ultrasonic cleaning are all performed at a frequency of 50Hz, wherein the duration of the first ultrasonic cleaning is 10min, and the duration of the second ultrasonic cleaning is the time for heating the second alkaline residual liquid from 30 ℃ to 80 ℃.
In addition, the coarse-mesh sieve in the step (2) is used for separating silicon materials and impurities, and the fine-mesh sieve is used for separating alkali liquor and impurities, the coarse-mesh sieve in the embodiment is 30 meshes, and the fine-mesh sieve is 200 meshes, and other embodiments can be selected according to actual conditions.
The invention has the advantages that alkali liquor is matched with sodium sulfate, ultrasonic cleaning is carried out for a plurality of times, and water injection and drainage are carried out while the third ultrasonic cleaning is carried out, so that the cleaning effect is improved; the alkali liquor is recycled, so that the use amount of the alkali liquor is reduced, and the cleaning cost is saved.
Example 2
A silicon material cleaning method comprises the following steps:
(1) adding liquid alkali into the silicon material, and stirring for 5min, wherein the liquid alkali is potassium hydroxide, and the concentration is 10 mol/L;
(2) sieving with a coarse sieve to obtain a first alkali washing silicon material and a first alkali residual liquid, and sieving with a fine sieve to obtain a second alkali residual liquid;
(3) adding the second alkaline residual liquid into the first alkaline silicon washing material, heating to 30 ℃, and performing first ultrasonic cleaning;
(4) adding sodium sulfate into the second alkali residual liquid, heating to 90 ℃ with the concentration of the sodium sulfate being 1mol/L, wherein the temperature rise range is 2 ℃/min, and continuously performing second ultrasonic cleaning in the heating process;
(5) and continuously injecting water into the second alkaline residual liquid, and simultaneously discharging the liquid, wherein the water injection speed v1 of the injected water is equal to the liquid outlet speed v2 of the discharged liquid, namely v1 is equal to v2, and the third ultrasonic cleaning is continuously performed in the process for 20min to obtain a second alkaline silicon washing material.
The remaining parameters correspond to those of example 1.
Example 3
A silicon material cleaning method comprises the following steps:
(1) adding liquid alkali into the silicon material, and stirring for 5min, wherein the liquid alkali is sodium hydroxide, and the concentration is 5 mol/L;
(2) sieving with a coarse sieve to obtain a first alkali washing silicon material and a first alkali residual liquid, and sieving with a fine sieve to obtain a second alkali residual liquid;
(3) adding the second alkaline residual liquid into the first alkaline silicon washing material, heating to 30 ℃, and performing first ultrasonic cleaning;
(4) adding sodium sulfate into the second alkali residual liquid, heating to 80 ℃ with the concentration of the sodium sulfate being 1mol/L, wherein the temperature rise range is 1 ℃/min, and continuously performing second ultrasonic cleaning in the heating process;
(5) and continuously injecting water into the second alkaline residual liquid, and simultaneously discharging the liquid, wherein the water injection speed v1 of the injected water is equal to the liquid outlet speed v2 of the discharged liquid, namely v1 is equal to v2, and the third ultrasonic cleaning is continuously performed in the process for 20min to obtain a second alkaline silicon washing material.
The remaining parameters correspond to those of example 1.
Example 4
This embodiment is substantially the same as embodiment 3 except that:
and (2) adopting sodium methoxide as alkali liquor in the step (1).
Example 5
This embodiment is substantially the same as embodiment 4 except that:
the heating process in the step (4) is as follows:
raising the temperature to 50 ℃ with the temperature rise amplitude of 1 ℃/min;
raising the temperature to 70 ℃ with the temperature rise amplitude of 0.5 ℃/min;
the temperature is increased to 80 ℃ with the temperature rise amplitude of 2 ℃/min.
Example 6
This embodiment is substantially the same as embodiment 5 except that:
the water injection speed v1 of the injected water and the liquid outlet speed v2 of the discharged liquid in the step (5) are 1.5 times, namely v1 is 1.5 v 2.
Comparative example 1
A silicon material cleaning method comprises the following steps:
(1) soaking the silicon material in 5mol/L sodium hydroxide, and continuously performing ultrasonic cleaning for 40 min;
(2) and then the silicon material is put into pure water to carry out ultrasonic cleaning for 20 min.
The ultrasonic cleaning in this comparative example was carried out at a frequency of 50 Hz.
Comparative example 2
This comparative example is substantially the same as comparative example 1 except that:
the concentration of sodium hydroxide was 18 mol/L.
Comparative example 3
This comparative example is substantially the same as example 6 except that:
sodium sulfate is not added in the step (4).
Comparative example 4
This comparative example is substantially the same as example 6 except that:
and (5) taking out the first alkaline silicon washing material, soaking the first alkaline silicon washing material in pure water, and performing ultrasonic cleaning for 20 min.
In order to make the present invention clearer, the silicon materials were cleaned by using the above examples and comparative example 1, respectively, using the same volume of liquid caustic soda, wherein the silicon materials were selected from small materials which were bought in a factory in Shanghai province in Jiangxi, the size of the single silicon material was substantially the same, and the amount of the silicon material used was different for each method. The surface of the silicon material is free of silicon nitride, impurity layers, alkaline spots and oxidation spots and is used as a finished product, the finished product is manually selected, the proportion of the finished product in the final product is calculated and used as the yield, and the result is shown in table 1.
TABLE 1
Referring to Table 1, comparing examples 1 to 3, it can be seen that when the liquid caustic soda is 10mol/L, the yield is greatly increased, but the cost of the liquid caustic soda is increased, and the pollution is also increased;
compared with the examples 3-6, the sodium methoxide, the sectional temperature rise and the water inlet speed increase have certain promotion effects on the yield, and certain positive effects are achieved;
comparing example 6 with comparative examples 1 and 2, it is known that the effect achieved by example 6 is much better than comparative example 1 when the same concentration of caustic soda is used, and that the yield is very high when a higher concentration of caustic soda is used, such as 18mol/L of sodium hydroxide in comparative example 2, but the amount of sodium hydroxide used is also greatly increased;
comparing example 6 with comparative example 3 and comparative example 4, it is found that the cleaning effect can be improved by ultrasonic cleaning with sodium sulfate and liquid caustic soda, and that the effect of ultrasonic cleaning by injecting water into the second alkaline residual liquid and discharging the liquid is better than that by directly injecting the liquid into pure water.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A silicon material cleaning method is characterized by comprising the following steps:
(1) adding liquid caustic soda into the silicon material, and stirring for 3-5 min;
(2) sieving with a coarse sieve to obtain a first alkali washing silicon material and a first alkali residual liquid, and sieving with a fine sieve to obtain a second alkali residual liquid;
(3) adding the second alkaline residual liquid into the first alkaline silicon washing material, heating to 30 ℃, and performing first ultrasonic cleaning;
(4) adding sodium sulfate into the second alkali residual liquid, heating to 80-90 ℃, and continuously performing second ultrasonic cleaning in the heating process;
(5) and continuously injecting water into the second alkali residual liquid, and simultaneously discharging liquid, and continuously performing third ultrasonic cleaning in the process to obtain a second alkali silicon cleaning material.
2. The silicon material cleaning method according to claim 1, wherein the alkali solution in the step (1) is sodium hydroxide, potassium hydroxide or sodium methoxide.
3. The silicon material cleaning method according to claim 1 or 2, wherein the concentration of the alkali liquor in the step (1) is 3-10 mol/L.
4. The silicon material cleaning method according to claim 1, wherein the coarse mesh in the step (2) is 20-100 meshes, and the fine mesh is 150-200 meshes.
5. The silicon material cleaning method according to claim 1, wherein the heating in the step (4) is carried out at a temperature rise range of 0.5-2 ℃/min.
6. The silicon material cleaning method according to claim 1 or 5, wherein the heating in the step (4) is carried out by the following temperature rise process:
raising the temperature to 50 ℃ with the temperature rise amplitude of 1 ℃/min;
raising the temperature to 70 ℃ with the temperature rise amplitude of 0.5 ℃/min;
raising the temperature to 80-90 ℃ at a temperature rise of 2 ℃/min.
7. The silicon material cleaning method according to claim 1, wherein the concentration of sodium sulfate in the step (4) is 1-5 mol/L.
8. The silicon material cleaning method according to claim 1, wherein the water injection speed of the injected water and the liquid outlet speed of the discharged liquid in the step (5) are equal.
9. The silicon material cleaning method according to claim 1, wherein the water injection speed of the injected water in the step (5) is 1.2 to 1.5 times of the liquid outlet speed of the discharged liquid.
10. The silicon material cleaning method according to claim 1, wherein the duration of the third ultrasonic cleaning in the step (5) is 10-20 min.
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| CN201911366795.7A CN111017929B (en) | 2019-12-26 | 2019-12-26 | Silicon material cleaning method |
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| CN201911366795.7A CN111017929B (en) | 2019-12-26 | 2019-12-26 | Silicon material cleaning method |
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| CN111017929A CN111017929A (en) | 2020-04-17 |
| CN111017929B true CN111017929B (en) | 2021-04-13 |
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| CN203803852U (en) * | 2014-01-28 | 2014-09-03 | 包头市山晟新能源有限责任公司 | Sheet silicon material washing device |
| RU2766149C2 (en) * | 2015-10-09 | 2022-02-08 | МИЛУОКИ СИЛИКОН, ЭлЭлСи | Purified silicon, as well as devices and systems for its production |
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