CN114606572A - Method for reducing volatilization of gallium dopant - Google Patents
Method for reducing volatilization of gallium dopant Download PDFInfo
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- CN114606572A CN114606572A CN202011450513.4A CN202011450513A CN114606572A CN 114606572 A CN114606572 A CN 114606572A CN 202011450513 A CN202011450513 A CN 202011450513A CN 114606572 A CN114606572 A CN 114606572A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B31/00—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor
- C30B31/04—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor by contacting with diffusion materials in the liquid state
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Abstract
The invention provides a method for reducing volatilization of gallium as a dopant. The method for reducing the volatilization of the gallium dopant comprises the following steps: (1) after partial silicon material is filled into the charging barrel, inserting a quartz tube into the silicon material, and then filling the rest silicon material into the outer side of the quartz tube; (2) and adding gallium into the quartz tube from the upper part of the quartz tube, and taking out the quartz tube after the gallium falls into the bottom of the quartz tube to realize the doping of the gallium. The method can effectively add the dopant into the middle lower part, simultaneously reduces the operation difficulty of personnel, and avoids gallium from volatilizing and adhering to the cylinder wall.
Description
Technical Field
The invention belongs to the field of photovoltaic energy manufacturing, and particularly relates to a method for reducing volatilization of a dopant gallium.
Background
At present, gallium-doped single crystals are popularized and used in the field of photovoltaic energy manufacturing, the inverse cutting proportion is reduced from 8.08% to 5.36%, and the hit rate of resistivity is improved from 30.56% to 57.38%. However, gallium is hard and brittle at low temperatures and melts as soon as it exceeds room temperature. And gallium is exposed to dry air, and the surface is contaminated by the formation of oxide films, especially tarnish in humid air. The solidification point of gallium is very low and the expansion rate is 3.1% when it is converted from liquid to solid.
The existing adding method is that solid gallium metal is weighed and then directly put into a quartz crucible filled with silicon materials or directly added into a re-adding charging barrel. Because the melting point of metal gallium is only 29.8 ℃, the problem that gallium metal is polluted or lost can occur; and as the diameter of the silicon charging barrel increases, the probability of gallium metal being polluted and falling and losing is increased continuously. And the method can not overcome the risk that the metal gallium reacts with quartz after being melted at high temperature or falls off after being changed into liquid in a re-feeding cylinder. The addition amount of gallium is seriously influenced, and finally, the quality of the product is influenced. In addition, the existing gallium doping mode cannot add gallium into the middle lower part of the charging barrel, and meanwhile, the risk that a dopant is stained on the inner wall of the charging barrel exists.
Therefore, the development of a method for reducing the volatilization of gallium as a dopant is the focus of research in the field.
Disclosure of Invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a method for reducing the volatilization of gallium as a dopant. The method can effectively add the dopant into the middle lower part, simultaneously reduces the operation difficulty of personnel, and avoids gallium from volatilizing and sticking to the cylinder wall.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for reducing volatilization of dopant gallium, the method comprising the steps of:
(1) after partial silicon material is filled into the charging barrel, inserting a quartz tube into the silicon material, and then filling the rest silicon material into the outer side of the quartz tube;
(2) and adding gallium into the quartz tube from the upper part of the quartz tube, and taking out the quartz tube after the gallium falls into the bottom of the quartz tube to realize the doping of the gallium.
The method for reducing the volatilization of the gallium dopant comprises the steps of filling a part of silicon material into a charging barrel, inserting a quartz tube, pouring a layer of crushed material, adding the dopant into the quartz tube, and burying the dopant in the silicon material after the quartz tube is pulled out. The adding mode can effectively add the dopant into the middle lower part, simultaneously reduces the operation difficulty of personnel, reduces volatilization and more accurately grasps the resistivity of the single crystal.
Preferably, in the step (1), the partial silicon material accounts for 1/4-2/3 of the total volume of the charging barrel, such as 1/4, 1/3, 1/2 or 2/3, preferably 1/3-1/2
Preferably, in the step (1), the insertion depth of the quartz tube is 1/20-1/10 of the thickness of the silicon material, and may be 1/20, 1/18, 1/16, 1/14, 1/12, 1/10 and the like.
Preferably, in the step (1), the diameter of the quartz tube is 1/6-1/3 of the diameter of the cylinder, such as 1/6, 1/5, 1/4, 1/3 and the like.
Preferably, in the step (1), the quartz tube is inserted to form a concentric circle with the barrel. The concentric circles are arranged so that the gallium is located in the center of the silicon material, and therefore the risks that the gallium volatilizes and adheres to the wall of the cylinder are further avoided.
Preferably, in the step (2), the gallium is added through a quartz funnel arranged above the quartz tube, so that the risks of gallium volatilization and adhesion to the wall of the tube are further avoided.
Preferably, the ratio of the tube section outer diameter of the quartz funnel to the inner diameter of the quartz tube is (0.9-1):1, and can be, for example, 0.9:1, 0.92:1, 0.94:1, 0.96:1, 0.98:1, 1:1, and the like.
Preferably, the length of the tube section of the quartz funnel is 1/20-1/10 of the length of the quartz tube, and can be 1/20, 1/18, 1/16, 1/14, 1/12, 1/10 and the like.
Preferably, in the step (2), when the gallium is added into the quartz tube from above the quartz tube, the inclination angle of the cylinder inserted into the quartz tube is 60 to 90 °, for example, 60 °, 65 °, 70 °, 75 °, 80 °, 85 °, 90 °.
In the present invention, the "inclined angle" means an acute angle formed by the axis of the charging barrel and the ground, when the gallium is fed into the quartz tube from above the quartz tube, the charging barrel inserted into the quartz tube preferably has a certain inclination angle, if the inclination angle is too small, the gallium is difficult to fall into the bottom of the charging barrel completely, and if the gallium is completely vertical (i.e. forms a right angle of 90 ° with the ground), the falling speed of the gallium is too fast, and the gallium is difficult to disperse uniformly.
In the step (2), the addition amount of gallium is preferably 0.006 to 0.01% of the total mass of the silicon material, and may be, for example, 0.006%, 0.007%, 0.008%, 0.009%, 0.01%, or the like.
Preferably, the method for reducing dopant gallium volatilization comprises the steps of:
(1) after a silicon material which accounts for 1/3-1/2 of the total volume of the charging barrel is filled into the charging barrel, a quartz tube is inserted into the silicon material, the quartz tube and the charging barrel form a concentric circle after being inserted, the insertion depth of the quartz tube is 1/20-1/10 of the thickness of the silicon material, and then the rest silicon material is filled outside the quartz tube;
(2) after a charging barrel inserted into a quartz tube is inclined by 60-90 degrees, gallium is added into the quartz tube through a quartz funnel arranged above the quartz tube, the ratio of the outer diameter of a tube section of the quartz funnel to the inner diameter of the quartz tube is (0.9-1):1, the length of the tube section of the quartz funnel is 1/20-1/10 of the length of the quartz tube, the gallium falls into the bottom of the quartz tube, and then the quartz tube is taken out, so that the doping of the gallium is realized.
Compared with the prior art, the invention has the following beneficial effects:
the adding mode of the invention can effectively add the dopant into the middle lower part, simultaneously reduces the operation difficulty of personnel, reduces volatilization, more accurately grasps the resistivity of the single crystal, and reduces the volatilization amount of gallium after 1h to be less than 0.006g, and the lowest volatilization amount can reach 0.001 g.
Drawings
FIG. 1 is a schematic view of an apparatus for use in the method of reducing dopant gallium volatilization of the present invention;
wherein, 1 is a charging barrel, 2 is a quartz tube, and 2 is a quartz funnel.
FIG. 2 is a schematic top view showing the positions of the quartz tube and the barrel in example 1;
wherein, 1 is a charging barrel, and 2 is a quartz tube.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
FIG. 1 is a schematic view of an apparatus for use in the method of reducing dopant gallium volatilization of the present invention; as shown in FIG. 1, a quartz tube 2 was inserted into a cylinder 1 containing a part of the silicon material, and the gallium was added through a quartz funnel 3 disposed above the quartz tube.
The sources of the devices in the following examples are as follows: the cylinder was purchased from Baokang (manufacturer), the quartz tube was purchased from Longshu quartz product (manufacturer: Longshu quartz product, model: 1.5-300mm), and the quartz funnel was purchased from Daiko quartz funnel (manufacturer: Mingkui, model: 60 mm/19).
The component sources in the following examples are as follows: silicon material is purchased from manufacturers (Daquan, Re-feeding materials), and metal gallium is purchased from manufacturers (Wuhan Tuo materials, purity 99.99999%).
Example 1
The embodiment provides a method for reducing volatilization of gallium dopant, which comprises the following steps:
(1) after 1/3 silicon material occupying the total volume of the charging barrel is charged into the charging barrel, a quartz tube is inserted into the silicon material, the quartz tube and the charging barrel form a concentric circle after being inserted (as shown in figure 2), the diameter of the quartz tube is 1/5 of the diameter of the charging barrel, the insertion depth of the quartz tube is 1/10 of the thickness of the silicon material, and the rest 2/3 silicon material is charged on the outer side of the quartz tube;
(2) after a charging barrel inserted into a quartz tube is inclined by 80 degrees, gallium accounting for 0.01 percent of the total mass of the silicon material is added into the quartz tube through a quartz funnel arranged above the quartz tube, the ratio of the outer diameter of a tube section of the quartz funnel to the inner diameter of the quartz tube is 0.95:1, the length of the tube section of the quartz funnel is 1/20 of the length of the quartz tube, and the gallium falls into the bottom of the quartz tube, then the quartz tube is taken out, and the doping of the gallium is realized.
Example 2
The embodiment provides a method for reducing volatilization of gallium dopant, which comprises the following steps:
(1) after 1/2 silicon materials occupying the total volume of the charging barrel are charged into the charging barrel, a quartz tube is inserted into the silicon materials, the quartz tube and the charging barrel form a concentric circle after being inserted, the diameter of the quartz tube is 1/4 of the diameter of the charging barrel, the insertion depth of the quartz tube is 1/5 of the thickness of the silicon materials, and the rest 1/2 silicon materials are charged on the outer side of the quartz tube;
(2) after a charging barrel inserted into a quartz tube is inclined by 70 degrees, gallium accounting for 0.01 percent of the total mass of the silicon material is added into the quartz tube through a quartz funnel arranged above the quartz tube, the ratio of the outer diameter of a tube section of the quartz funnel to the inner diameter of the quartz tube is 0.95:1, the length of the tube section of the quartz funnel is 1/15 of the length of the quartz tube, and the gallium falls into the bottom of the quartz tube, then the quartz tube is taken out, and the doping of the gallium is realized.
Example 3
This example provides a method for reducing dopant gallium volatilization, which differs from example 1 only in that in step (1), the portion of silicon material occupies 1/4 of the total volume of the cartridge, and the other steps are the same as example 1.
Example 4
This example provides a method for reducing dopant gallium volatilization, which differs from example 1 only in that in step (1), the portion of silicon material occupies 2/3 of the total volume of the cartridge, and the other steps are the same as example 1.
Example 5
In the step (1), the insertion position of the quartz tube is as follows: the circle center of the quartz tube is located at the circle center of the charging barrel and the barrel wall 1/2 of the charging barrel, and other steps are the same as those in embodiment 1.
Example 6
This example provides a method for reducing volatilization of gallium as dopant, which is different from example 1 only in that in step (1), no quartz funnel is disposed above the quartz tube, in step (2), gallium metal is directly poured from the tube mouth of the quartz tube, and other steps are the same as example 1.
Example 7
This example provides a method for reducing volatilization of gallium as a dopant, and is different from example 1 only in that, in step (2), when gallium is introduced into a quartz tube from above the quartz tube, the tilt angle of a cartridge inserted into the quartz tube is 90 °, and other steps are the same as example 1.
Example 8
This example provides a method for reducing volatilization of gallium as a dopant, and is different from example 1 only in that, in step (2), when gallium is introduced into a quartz tube from above the quartz tube, the tilt angle of a cartridge inserted into the quartz tube is 45 °, and other steps are the same as example 1.
Comparative example 1
The present comparative example provides a method of reducing volatilization of dopant gallium, the method comprising the steps of:
(1) after the entire silicon charge was loaded into the barrel, a quartz tube was inserted 2/3 times the thickness of the silicon charge;
(2) after a charging barrel inserted into a quartz tube is inclined by 80 degrees, gallium accounting for 0.01 percent of the total mass of the silicon material is added into the quartz tube through a quartz funnel arranged above the quartz tube, the ratio of the outer diameter of a tube section of the quartz funnel to the inner diameter of the quartz tube is 0.95:1, the length of the tube section of the quartz funnel is 1/20 of the length of the quartz tube, and the gallium falls into the bottom of the quartz tube, then the quartz tube is taken out, and the doping of the gallium is realized.
Performance testing
After 1h, respectively testing the gallium volatilization amount of the above examples 1-8 and the comparative examples 1-2 at the material cylinder opening by using an oscillometric polarograph, measuring each group of samples for 10 times, and taking an average value, wherein the specific test method refers to the method for measuring trace crops in air by using an oscillometric polarography;
the specific test results are shown in table 1 below:
TABLE 1
| Group of | Amount of volatile gallium |
| Example 1 | 0.001g |
| Example 2 | 0.001g |
| Example 3 | 0.001g |
| Example 4 | 0.004g |
| Example 5 | 0.006g |
| Example 6 | 0.002g |
| Example 7 | 0.001g |
| Example 8 | 0.002g |
| Comparative example 1 | 0.009g |
As can be seen from the test data in Table 1, the volatilization amount of gallium after 1 hour is reduced to below 0.006g, and the lowest amount can reach 0.001g by the doping method of the invention after 1 hour. The adding mode of the invention can effectively add the dopant into the middle lower part, simultaneously reduces the operation difficulty of personnel, reduces volatilization and more accurately grasps the resistivity of the single crystal.
The applicant states that the present invention is illustrated by the above examples to describe the method of reducing the dopant gallium volatilization, but the present invention is not limited to the above examples, i.e. it does not mean that the present invention must be implemented by relying on the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A method of reducing dopant gallium volatility, said method comprising the steps of:
(1) after partial silicon material is filled into the charging barrel, inserting a quartz tube into the silicon material, and then filling the rest silicon material into the outer side of the quartz tube;
(2) and adding gallium into the quartz tube from the upper part of the quartz tube, and taking out the quartz tube after the gallium falls into the bottom of the quartz tube to realize the doping of the gallium.
2. The method for reducing volatilization of gallium dopant according to claim 1, characterized in that in step (1), the partial silicon material accounts for 1/4-2/3, preferably 1/3-1/2 of the total volume of the barrel.
3. The method for reducing volatilization of gallium dopant according to claim 1 or 2, wherein in step (1), the quartz tube is inserted to a depth of 1/20-1/10 of the thickness of the silicon material.
4. The method for reducing dopant gallium volatilization according to any one of claims 1 to 3, wherein in step (1), the diameter of the quartz tube is 1/6-1/3 of the diameter of the barrel.
5. The method for reducing dopant gallium volatilization according to any one of claims 1 to 4, wherein in step (1), the quartz tube is inserted to form a concentric circle with the cartridge.
6. The method for reducing dopant gallium volatilization according to any one of claims 1-5, wherein in step (2), the gallium is added through a quartz funnel disposed above a quartz tube.
7. The method for reducing dopant gallium volatilization according to claim 6, wherein the ratio of the outer diameter of the tube section of the quartz funnel to the inner diameter of the quartz tube is (0.9-1): 1;
preferably, the length of the tube section of the quartz funnel is 1/20-1/10 of the length of the quartz tube.
8. The method for reducing volatilization of gallium dopant according to any one of claims 1 to 7, wherein in the step (2), when the gallium is fed into the quartz tube from above the quartz tube, the angle of inclination of the barrel inserted into the quartz tube is 60 to 90 °.
9. The method for reducing volatilization of gallium dopant according to any one of claims 1 to 8, wherein in step (2), the amount of gallium added is 0.006 to 0.01% of the total mass of the silicon material.
10. The method of reducing dopant gallium volatilization according to any of claims 1-9, wherein the method of reducing dopant gallium volatilization comprises the steps of:
(1) after a silicon material which accounts for 1/3-1/2 of the total volume of the charging barrel is filled into the charging barrel, a quartz tube is inserted into the silicon material, the quartz tube and the charging barrel form a concentric circle after being inserted, the insertion depth of the quartz tube is 1/10-1/5 of the thickness of the silicon material, and then the rest silicon material is filled outside the quartz tube;
(2) after a charging barrel inserted into a quartz tube is inclined by 60-90 degrees, gallium is added into the quartz tube through a quartz funnel arranged above the quartz tube, the ratio of the outer diameter of a tube section of the quartz funnel to the inner diameter of the quartz tube is (0.9-1):1, the length of the tube section of the quartz funnel is 1/20-1/10 of the length of the quartz tube, the gallium falls into the bottom of the quartz tube, and then the quartz tube is taken out, so that the doping of the gallium is realized.
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| JP2010222162A (en) * | 2009-03-23 | 2010-10-07 | Covalent Materials Corp | Doping agent supply device and apparatus for producing semiconductor single crystal |
| CN102409395A (en) * | 2011-11-15 | 2012-04-11 | 浙江长兴众成电子有限公司 | Gallium element doping device and method for Czochralski silicon |
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| CN111663177A (en) * | 2020-05-29 | 2020-09-15 | 包头美科硅能源有限公司 | Gallium metal adding method of gallium-doped monocrystalline silicon and gallium metal placing structural body |
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2020
- 2020-12-09 CN CN202011450513.4A patent/CN114606572B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2010222162A (en) * | 2009-03-23 | 2010-10-07 | Covalent Materials Corp | Doping agent supply device and apparatus for producing semiconductor single crystal |
| CN101805925A (en) * | 2010-02-20 | 2010-08-18 | 西安隆基硅材料股份有限公司 | Gallium and indium doped single crystal silicon material for solar battery and preparation method thereof |
| CN102409395A (en) * | 2011-11-15 | 2012-04-11 | 浙江长兴众成电子有限公司 | Gallium element doping device and method for Czochralski silicon |
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