CN113526510A - Method for reducing radiation heat loss of polycrystalline silicon reduction furnace and application - Google Patents
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Abstract
The invention discloses a method for reducing the radiant heat loss of a polycrystalline silicon reduction furnace and application, belonging to the technical field of polycrystalline silicon production, wherein a quartz ceramic lining material is coated on the inner wall of the furnace body of the polycrystalline silicon reduction furnace, the quartz ceramic lining material is prepared by taking amorphous quartz or crystalline quartz or a mixture of the amorphous quartz and the crystalline quartz as a raw material through a series of processes of grinding, pulping, blank forming, sintering, cold processing and the like, and more than one layer of quartz ceramic lining material consisting of different raw materials is coated on the inner wall of the furnace body of the polycrystalline silicon reduction furnace; the quartz ceramic material adopted by the invention has the advantages of low thermal conductivity, small expansion coefficient, high temperature resistance, good thermal stability and lower cost, can replace the existing precious metal plating materials such as gold, silver and the like, is beneficial to reducing the radiation heat loss of the polysilicon reduction furnace, saves the power consumption, thereby reducing the production cost and improving the production efficiency.
Description
Technical Field
The invention belongs to the technical field of polycrystalline silicon production, and particularly relates to a method for reducing the radiant heat loss of a polycrystalline silicon reduction furnace and application thereof.
Background
At present, the main process for producing polycrystalline silicon in the world is the modified siemens method, and the yield accounts for 70 percent of the total yield in the world. The polysilicon reduction furnace is one of core devices for producing polysilicon by an improved Siemens method, and the high power consumption of the polysilicon reduction furnace is one of the main technical problems which hinder the development of the polysilicon reduction furnace. Therefore, the research and development of the high-efficiency and energy-saving polycrystalline silicon reduction furnace is the key for improving the competitiveness of the polycrystalline silicon production by the Siemens method.
The temperature of the silicon rod in the polysilicon reducing furnace is one of important technological parameters for polysilicon production, and the technology requires that the surface temperature of the silicon rod is controlled to be about 1100 ℃ so as to ensure that trichlorosilane is reduced and deposited on the surface of the silicon rod under the action of hydrogen. For the polysilicon reduction furnace, the energy consumption mainly comes from the radiation heat loss between the silicon rod and the wall of the water cooler, and accounts for about 70 percent of the total energy loss, so that the reduction of the radiation heat loss of the polysilicon reduction furnace is one of important ways for realizing the improvement of energy conservation and consumption reduction by the Siemens method.
The inner wall of the improved Siemens method polycrystalline silicon reduction furnace has a very severe operating environment, the surface temperature of the silicon rod reaches 1100 ℃ in the operating process, and the silicon rod continuously carries out heat radiation in all directions, so that the temperature of the furnace body is increased. High-pressure cooling water in the reducing furnace wall cooling water jacket is forced to circulate by a water pump to continuously take away heat transferred inside the furnace body, and the temperature of the furnace wall of the bell jar type reducing furnace is maintained within the range of 100-200 ℃ so as to reduce the deposition of silicon powder on the surface of the inner wall of the reducing furnace. The trichlorosilane and the hydrogen chloride in the furnace are strong corrosive gases. These two extreme conditions, high temperature and strong corrosive gases, put severe demands on furnace wall materials. At present, the aims of high-temperature corrosion resistance and infrared radiation reflection are achieved by plating pure silver or even pure gold on stainless steel. The gold has good chemical stability, is a very good infrared reflection material, and can reflect infrared radiation to reduce the radiation heat loss in the reduction furnace. Silver has good chemical stability, but the infrared band reflection capability is not high. The hardness of gold and silver is very low, and when the reduction furnace is in a rod falling state in the operation process, the gold and silver layers are easily scraped and lost if the reduction furnace is rubbed against the furnace wall. In addition, gold and silver are both noble metals, and the recoating material is high in cost, which undoubtedly increases the production cost.
By adopting the existing coating technology, the high-reflectivity metal materials such as gold and silver are coated on the inner wall of the reduction furnace, the infrared reflection capability of the inner wall is improved, the radiation heat loss in the polysilicon reduction furnace can be effectively reduced to a certain extent, but the coating technology has the following problems: (1) the cost of noble metals such as gold, silver and the like is high, and the processing technology of the existing gold, silver or gold and silver composite coating is difficult; (2) the gold and silver coating is adopted to save energy, and the high infrared reflection capability of noble metals such as gold and silver is mainly utilized to reflect the infrared heat radiation emitted by the polycrystalline silicon rod of the heating body. The thickness of the gold and silver coating is generally controlled to be 10 nm-50 nm, a cooling water jacket is arranged outside the wall of the reduction furnace, circulating water in the jacket is controlled to be 100-200 ℃, therefore, the temperature of the coating is lower than 200 ℃, and the energy-saving mechanism can be called as cold reflection effect. Along with the middle and later periods of the operation of the polycrystalline silicon reduction furnace, silicon powder is formed and attached to the surface of the coating, so that the reflection capacity of the silver or silver composite coating material can be greatly reduced, and the energy-saving effect cannot be achieved; (3) the hardness of the precious metal materials such as gold and silver is low, and when the silicon rod is accidentally overturned in the operation of the reduction furnace, the silver or silver composite coating is easily scraped and lost, so that the production cost is increased undoubtedly.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for reducing the radiation heat loss of a polycrystalline silicon reduction furnace, which adopts a quartz ceramic lining to replace the existing precious metal plating materials such as gold, silver and the like, has low cost, strong high-temperature corrosion resistance and high infrared reflectivity, is favorable for reducing the radiation heat loss of the polycrystalline silicon reduction furnace and saving reduction power consumption, thereby reducing the production cost.
The technical scheme of the invention is as follows: a method for reducing radiation heat loss of a polycrystalline silicon reduction furnace is characterized in that a quartz ceramic lining material is coated on the inner wall of the furnace body of the polycrystalline silicon reduction furnace, and the quartz ceramic lining material is prepared by taking amorphous quartz or crystalline quartz or a mixture of the amorphous quartz and the crystalline quartz as a raw material through a series of processes such as grinding, pulping, blank forming, sintering, cold machining and the like. More than one layer of quartz ceramic lining material which is composed of different raw materials is coated on the inner wall of the furnace body of the polysilicon reduction furnace. For example, a layer of quartz ceramic material made of amorphous quartz can be coated, and then a layer of quartz ceramic material made of crystalline quartz or quartz ceramic material made of amorphous quartz and crystalline quartz can be coated on the quartz ceramic material.
The particle size range of the quartz ceramic lining material is 50 nm-300 mu m, the porosity is 1% -90%, the purity of silicon dioxide is more than 99.99%, the melting point of the quartz ceramic lining material is 1723 ℃, and the density is 2.2 g/cm3Coefficient of thermal expansion of 12.3X 10-6 K-1The thermal conductivity is 0.2 to 1.6W/m ∙ K.
The quartz ceramic lining material is obtained by using a colloid treatment method, and the method comprises the following specific steps:
grinding unprocessed amorphous or crystalline quartz to a particle size of 50 nm-300 mu m, and then dispersing the ground quartz particles into a colloidal solution;
secondly, molding the quartz particles dispersed in the colloidal solution into a molding material or a panel, and then drying, sintering and annealing;
and subjecting the prepared profile or panel to machining (e.g., polishing) or structural modification to introduce locking elements or other features for installation into a polysilicon reduction furnace. Thereby obtaining the quartz ceramic lining material.
The polycrystalline silicon reduction furnace is an improved Siemens method polycrystalline silicon reduction furnace.
The method for reducing the radiation heat loss of the polycrystalline silicon reduction furnace is applied to the chemical vapor deposition of the improved Siemens method.
The invention is characterized in that: according to the invention, the quartz ceramic material is used as the lining material of the polycrystalline silicon reduction furnace, and due to the excellent high-temperature corrosion resistance, the quartz ceramic lining is not in contact with SiHCl in a high-temperature environment above 600 DEG C3HCl and SiCl4Strong corrosive gas in equal furnaceThe body is chemically reacted, and no metal impurities are introduced. The quartz ceramic material can reflect part of infrared radiation from the silicon rod back, the quartz ceramic lining absorbs the infrared radiation from the polycrystalline silicon rod of the heating body, the surface temperature of the quartz ceramic lining is increased, and the high-temperature surface of the quartz ceramic lining faces the heated polycrystalline silicon rod to emit thermal radiation by utilizing the heat emission effect, so that the radiation heat loss of the polycrystalline silicon reduction furnace is reduced. Quartz ceramics have a so-called red hardness, i.e. the hardness does not substantially change at temperatures below 600 ℃. The coefficient of friction of quartz ceramics is as low as 0.4. These two points are very important for the lining material of the polysilicon reduction furnace. When the silicon rod is accidentally overturned to scrape the furnace wall, the high hardness of the quartz ceramic enables the lining of the reduction furnace to bear high impact force. Meanwhile, the low friction coefficient can reduce the shearing force acting on the lining interface caused by impact, and the quartz ceramic lining and the stainless steel furnace wall material have strong binding force, so that the phenomenon that the quartz ceramic lining is easily scraped off like gold and silver coating materials can be avoided.
Compared with the prior art, the invention has the beneficial effects that:
the quartz ceramic material adopted by the invention has the advantages of low thermal conductivity, small expansion coefficient, high temperature resistance, good thermal stability and lower cost, can replace the existing precious metal plating materials such as gold, silver and the like, is beneficial to reducing the radiation heat loss of the polysilicon reduction furnace, saves the power consumption, thereby reducing the production cost and improving the production efficiency.
Drawings
FIG. 1 is a schematic view of a basic structure of a multi-layer lining of a polysilicon reduction furnace according to the present invention;
FIG. 2 is a graph illustrating the reduction of radiant heat loss in a polysilicon reduction furnace according to the present invention;
FIG. 3 is a graph showing the reduction of energy consumption per kilogram of polysilicon product according to the present invention.
Detailed Description
The invention is further described with reference to the following drawings and detailed description.
Example 1: and the inner wall of the polysilicon reduction furnace is subjected to mechanical polishing, cleaning by an organic solvent and pure water, drying and then is ready for plating. The system is vacuumized and reaches a predetermined vacuum degree (10)-4About Pa),an infrared heating body is used for heating the furnace wall to 300 ℃ for baking and degassing. And introducing argon to carry out ion glow discharge cleaning on the inner wall of the reduction furnace after degassing is finished. The manufacturing procedure of the quartz ceramic lining can use colloid treatment, and comprises the following specific steps: mixing raw amorphous quartz (SiO)2Purity 99.99%) until the diameter is 50 nm-300 μm, the porosity is 1% -90%, the melting point is 1723 ℃, and the density is 2.2 g/cm3Coefficient of thermal expansion of 12.3X 10-6 K-1The thermal conductivity is 0.2-1.6W/m ∙ K, and the formed ground quartz particles are dispersed in the colloidal solution. The milled quartz particles are molded into panels, then dried, sintered and annealed, and the prepared panels are machined and polished to incorporate locking elements or other features for installation into a polysilicon reduction furnace, and the quartz ceramic lining is prepared.
The quartz ceramic lining prepared in the embodiment is used for the trichlorosilane hydrogen reduction process of a polysilicon reduction furnace, the diameter of the reduction furnace is 1600 mm, the number of silicon rods is 12 pairs, the height of the silicon rods is 2400 mm, the temperature of the silicon rods is 1100 ℃, the feeding temperature is 120 ℃, the temperature of circulating water of a jacket of the reduction furnace is 100 ℃, the operating pressure is 0.5 MPa, and SiHCl is3Feed gas flow rate is 1015 kg/H, H2/SiHCl3And (5) =3:1 (volume ratio), and performing trichlorosilane hydrogen reduction reaction.
Comparing the radiant heat loss in the polysilicon reduction furnace, a 20 mm quartz ceramic lining prepared by using amorphous quartz as a raw material is installed, as shown in figure 2. When the radius of the silicon rod grows to 7 cm, the radiation heat loss in the reducing furnace is reduced from 1232 kW to 1043 kW, and the radiation heat loss is reduced by 15%.
When the inner wall of the polycrystalline silicon reduction furnace is coated with a layer of quartz ceramic lining, the quartz ceramic material has the advantages of low thermal conductivity, small expansion coefficient, high temperature resistance, good thermal stability, lower cost and the like, has similar performance to a heat insulating material, limits the heat transfer through the ceramic lining, and reduces the heat loss taken away by a cooling water jacket of the reduction furnace wall. Meanwhile, the quartz ceramic lining absorbs infrared radiation from the polycrystalline silicon rod of the heating body, the surface temperature of the quartz ceramic lining is increased, and the surface of the high-temperature quartz ceramic lining faces the heated polycrystalline silicon rod to emit thermal radiation by utilizing the thermal emission effect of the quartz ceramic lining, so that the reduction of the radiation heat loss of the polycrystalline silicon reduction furnace is facilitated. Compared with the existing gold, silver and other noble metal coating technologies, the energy-saving mechanism of the method is mainly based on the high infrared reflection capability of gold, silver and other noble metal materials, and the energy-saving mechanism can be called as a cold reflection effect. By utilizing the quartz ceramic lining and based on the thermal emission effect, the manufacturing cost can be reduced, and the energy efficiency of the polycrystalline silicon reduction furnace can be stably improved.
Example 2
And the inner wall of the polysilicon reduction furnace is subjected to mechanical polishing, cleaning by an organic solvent and pure water, drying and then is ready for plating. The system is vacuumized and reaches a predetermined vacuum degree (10)-4Pa or so), heating the furnace wall to 300 ℃ by using an infrared heating element, and baking to degas. And introducing argon to carry out ion glow discharge cleaning on the inner wall of the reduction furnace after degassing is finished. The quartz ceramic liner manufacturing process may use a colloidal treatment comprising: raw crystalline quartz (SiO)2Purity 99.99%) until the diameter is 50 nm-300 μm, the porosity is 1% -90%, the melting point is 1723 ℃, and the density is 2.2 g/cm3Coefficient of thermal expansion of 12.3X 10-6 K-1The thermal conductivity is 0.2-1.6W/m ∙ K, and the formed ground quartz particles are dispersed in the colloidal solution. The milled quartz particles may be molded into panels and then dried, sintered, and annealed. The prepared panel is machined and polished to incorporate locking elements or other features to facilitate its installation into a polysilicon reduction furnace and the quartz ceramic lining is prepared.
The quartz ceramic lining prepared in the embodiment is used for the trichlorosilane hydrogen reduction process of a polysilicon reduction furnace, the diameter of the reduction furnace is 1600 mm, the number of silicon rods is 12 pairs, the height of the silicon rods is 2400 mm, the temperature of the silicon rods is 1100 ℃, the feeding temperature is 120 ℃, the temperature of circulating water of a jacket of the reduction furnace is 100 ℃, the operating pressure is 0.5 MPa, and SiHCl is3Feed gas flow rate is 1015 kg/H, H2/SiHCl3And (5) =3:1 (volume ratio), and performing trichlorosilane hydrogen reduction reaction.
Comparing the radiant heat loss in the polysilicon reduction furnace, a layer of 30 mm quartz ceramic lining prepared by taking crystalline quartz as a raw material is arranged, and is shown in figure 2. When the radius of the silicon rod grows to 7 cm, the radiation heat loss in the reducing furnace is reduced from 1232 kW to 859 kW, and the radiation heat loss is reduced by 30%. Under the conditions of the example, the energy consumption per kilogram of polysilicon products is reduced from 55 kWh/kg-Si to 36 kWh/kg-Si, as shown in figure 3.
Example 3
And the inner wall of the polysilicon reduction furnace is subjected to mechanical polishing, cleaning by an organic solvent and pure water, drying and then is ready for plating. The system is vacuumized and reaches a predetermined vacuum degree (10)-4Pa or so), an infrared heating element is used for heating the furnace wall to the temperature of 300-600 ℃ for baking and degassing. And introducing argon to carry out ion glow discharge cleaning on the inner wall of the reduction furnace after degassing is finished. The quartz ceramic liner manufacturing process may use a colloidal treatment comprising: mixing raw amorphous and crystalline quartz (SiO)2Purity 99.99%) until the diameter is 50 nm-300 μm, the porosity is 1% -90%, the melting point is 1723 ℃, and the density is 2.2 g/cm3Coefficient of thermal expansion of 12.3X 10-6K-1The thermal conductivity is 0.2-1.6W/m ∙ K, and the formed ground quartz particles are dispersed in the colloidal solution. The milled quartz particles may be molded into panels and then dried, sintered, and annealed. The prepared panel is machined and polished to incorporate locking elements or other features to facilitate its installation into a polysilicon reduction furnace and the quartz ceramic lining is prepared.
The quartz ceramic lining prepared in the embodiment is used for the trichlorosilane hydrogen reduction process of a polysilicon reduction furnace, the diameter of the reduction furnace is 1600 mm, the number of silicon rods is 12 pairs, the height of the silicon rods is 2400 mm, the temperature of the silicon rods is 1100 ℃, the feeding temperature is 120 ℃, the temperature of circulating water of a jacket of the reduction furnace is 100 ℃, the operating pressure is 0.5 MPa, and SiHCl is3Feed gas flow rate is 1015 kg/H, H2/SiHCl3And (5) =3:1 (volume ratio), and performing trichlorosilane hydrogen reduction reaction.
Comparing the radiant heat loss in the polysilicon reducing furnace, as shown in fig. 1, a 30 mm quartz ceramic layer prepared from crystalline quartz is mounted, and on the basis, a 20 mm quartz ceramic layer prepared from a mixture of amorphous and crystalline quartz is mounted to form a 50 mm thick mixed double-layer ceramic lining, as shown in fig. 2. When the radius of the silicon rod grows to 7 cm, the radiation heat loss in the reducing furnace is reduced from 1232 kW to 629 kW, and the radiation heat loss is reduced by 49%.
The method according to the embodiment can manufacture the lining coating of the reducing furnace, and the lining coating of the reducing furnace also meets related technical indexes through performance tests, and has the advantages and obvious technical and economic effects compared with the prior art.
Although the embodiments of the present invention have been described in conjunction with the accompanying drawings, those skilled in the art may make various modifications and variations without departing from the spirit and scope of the invention, and such modifications and variations fall within the scope defined by the appended claims.
Claims (6)
1. The method for reducing the radiation heat loss of the polycrystalline silicon reduction furnace is characterized in that a quartz ceramic lining material is coated on the inner wall of the furnace body of the polycrystalline silicon reduction furnace, and the quartz ceramic lining material is prepared by taking amorphous quartz or crystalline quartz or a mixture of the amorphous quartz and the crystalline quartz as a raw material.
2. The method for reducing the radiant heat loss of the polycrystalline silicon reduction furnace according to claim 1, characterized in that: more than one layer of quartz ceramic lining material which is composed of different raw materials is coated on the inner wall of the furnace body of the polysilicon reduction furnace.
3. The method for reducing the radiant heat loss of the polycrystalline silicon reduction furnace according to claim 1, characterized in that: the particle size range of the quartz ceramic lining material is 50 nm-300 mu m, the porosity is 1% -90%, the purity of silicon dioxide is more than 99.99%, the melting point of the quartz ceramic lining material is 1723 ℃, and the density is 2.2 g/cm3Coefficient of thermal expansion of 12.3X 10-6 K-1The thermal conductivity is 0.2 to 1.6W/m ∙ K.
4. The method for reducing the radiant heat loss of the polycrystalline silicon reduction furnace according to claim 1, characterized in that: the quartz ceramic lining material is obtained by using a colloid treatment method, and the method comprises the following specific steps:
grinding unprocessed amorphous or crystalline quartz to a particle size of 50 nm-300 mu m, and then dispersing the ground quartz particles into a colloidal solution;
secondly, molding the quartz particles dispersed in the colloidal solution into a molding material or a panel, and then drying, sintering and annealing;
and thirdly, machining or modifying the structure of the prepared section or panel to introduce a locking element, thereby obtaining the quartz ceramic lining material.
5. The method for reducing the radiant heat loss of the polycrystalline silicon reduction furnace according to claim 1, characterized in that: the polycrystalline silicon reduction furnace is an improved Siemens method polycrystalline silicon reduction furnace.
6. The method for reducing the radiant heat loss of the polycrystalline silicon reduction furnace, according to claims 1 to 5, is applied to the chemical vapor deposition of the modified Siemens method.
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| CN113816383A (en) * | 2021-11-12 | 2021-12-21 | 昆明学院 | High-purity quartz silicon core for improving energy efficiency of polycrystalline silicon reduction furnace |
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