CN111690924A - Reduction furnace inner wall treatment device and method - Google Patents
Reduction furnace inner wall treatment device and method Download PDFInfo
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- CN111690924A CN111690924A CN202010541115.7A CN202010541115A CN111690924A CN 111690924 A CN111690924 A CN 111690924A CN 202010541115 A CN202010541115 A CN 202010541115A CN 111690924 A CN111690924 A CN 111690924A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
- C23C24/04—Impact or kinetic deposition of particles
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- C—CHEMISTRY; METALLURGY
- 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
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
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- Coating By Spraying Or Casting (AREA)
Abstract
The invention provides a device and a method for treating the inner wall of a reduction furnace, which relate to the technical field of polycrystalline silicon equipment, and comprise a bell jar, a rotating mechanism, a magnetic induction heating assembly and a cold gas power spray gun; the bell jar is provided with a closed accommodating space; the rotating mechanism is in transmission connection with the bell jar and is used for driving the bell jar to rotate; the magnetic induction heating assembly comprises a high-frequency coil, and the high-frequency coil is arranged in the accommodating space and used for heating the inner wall surface of the bell jar to a preset temperature range; the cold gas power spray gun is arranged in the accommodating space and is used for spraying powder to the inner wall surface of the bell jar. Through this reducing furnace inner wall processing apparatus, solved the cold gas dynamic spraying method that exists among the prior art, the bell jar adopts the great stainless steel of hardness more, the higher technical problem of requirement to the spraying condition.
Description
Technical Field
The invention relates to the technical field of polycrystalline silicon equipment, in particular to a device and a method for treating the inner wall of a reduction furnace.
Background
Crystalline silicon is a basic material in the microelectronics industry and the photovoltaics industry, and the improved siemens method is the current mainstream method for preparing polycrystalline silicon. The improved Siemens method is characterized in that: in a bell-jar Chemical Vapor Deposition (CVD) reactor (the industry term is polysilicon reduction furnace), a fine silicon core which is electrified and self-heated to 950-1150 ℃ is used as a deposition carrier, trichlorosilane and hydrogen which are introduced into the polysilicon reduction furnace generate hydrogen reduction reaction on the surface of the hot silicon core, the reduced silicon is deposited on the surface of a silicon core, the diameter of the silicon core is gradually increased along with the hydrogen reduction reaction until the silicon core reaches the specified size, and finally the silicon core is extracted in the form of a polysilicon rod.
The polysilicon reduction furnace is mainly made of stainless steel, and in order to avoid the problem that the creep deformation of the stainless steel material fails due to overhigh temperature of the inner wall in the operation process of the polysilicon reduction furnace, low-temperature water is usually introduced into a jacket between the outer wall and the inner wall for cooling, so that the temperature of the inner wall is kept below 300 ℃. During the operation process of the polysilicon reduction furnace, a large amount of infrared electromagnetic waves are emitted from the surface of the silicon rod, almost all the infrared electromagnetic waves reaching the surface of the inner wall are absorbed and converted into internal heat energy of the inner wall, and then the internal heat energy is conducted to high-heat-capacity low-temperature cooling water. According to statistics, the heat taken away by the jacket cooling water accounts for more than 60% of the total input energy of the polycrystalline silicon reduction furnace. At present, a precious metal coating mainly containing silver is prepared on the inner wall of the polycrystalline silicon reduction furnace, and the excellent infrared electromagnetic wave reflection performance of the precious metal coating is utilized, so that the reflectivity of the inner wall of the reduction furnace to infrared radiation is improved, the heat loss and the input energy are reduced, and the purpose of saving energy of the polycrystalline silicon reduction furnace is achieved.
The cold gas dynamic spraying method is a novel preparation technology of an energy-saving coating on the inner wall of a polysilicon reduction furnace, and is characterized in that: the metal powder is accelerated to supersonic speed by the heated compressed gas, and at the temperature lower than the melting point of the compressed gas, the metal powder impacts the surface of the substrate to form a coating on the surface of the substrate through mechanical interlocking action and violent elastic deformation between the metal powder and the substrate. Because the matrix mostly adopts stainless steel with higher hardness, and the temperature of the inner wall of the bell jar is normal temperature in the spraying process, the high-strength coating can be obtained only by needing higher spraying conditions (spraying temperature and spraying pressure), and the processing cost is increased undoubtedly.
Disclosure of Invention
The invention aims to provide a device and a method for treating the inner wall of a reduction furnace, which are used for solving the technical problem that the requirement on spraying conditions is high for obtaining a high-strength coating in a cold gas dynamic spraying method in the prior art.
In a first aspect, an embodiment of the present invention provides a reducing furnace inner wall processing apparatus, including: the device comprises a bell jar, a rotating mechanism, a magnetic induction heating assembly and a cold gas power spray gun.
The bell jar is provided with a closed accommodating space.
The rotating mechanism is in transmission connection with the bell jar and is used for driving the bell jar to rotate.
The magnetic induction heating assembly comprises a high-frequency coil, and the high-frequency coil is arranged in the accommodating space and used for heating the inner wall surface of the bell jar to a preset temperature range.
The cold gas power spray gun is arranged in the accommodating space, rotates relative to the bell jar and is used for spraying powder to the inner wall surface of the bell jar.
Furthermore, the high-frequency coil is of a hollow tubular structure, one end of the hollow tubular structure is used for being connected with a liquid inlet pipeline, and the other end of the hollow tubular structure is used for being connected with a liquid outlet pipeline.
Further, the magnetic shielding assembly is also included.
The magnetic shielding assembly comprises a magnetic shielding cover used for absorbing an electromagnetic field generated by the high-frequency coil, and the magnetic shielding cover is positioned in the accommodating space.
The high-frequency coil is located between the bell jar and an outer peripheral side of the magnetic shield.
The cold gas power spray gun comprises a gun body part and a spraying part, wherein the gun body part is positioned in the magnetic shielding cover, and the spraying part penetrates out of the magnetic shielding cover and faces the inner wall surface of the bell jar.
Furthermore, the magnetic shielding case comprises an inner magnetic shielding case and an outer magnetic shielding case, and the inner magnetic shielding case and the outer magnetic shielding case enclose a cavity.
A cooling pipe is arranged in the cavity, one end of the cooling pipe is used for being connected with a liquid inlet pipeline, and the other end of the cooling pipe is used for being connected with a liquid outlet pipeline; or the cavity is provided with an inlet and an outlet, the inlet is used for being connected with a liquid inlet pipeline, and the outlet is used for being connected with a liquid outlet pipeline.
Preferably, the outer diameter of the cooling pipe is 5-30 mm, and the inner diameter of the cooling pipe is 2-20 mm.
Furthermore, the high-frequency coils are in multiple groups, the multiple groups of high-frequency coils are sequentially and fixedly wound on the outer peripheral side of the outer magnetic shielding case from top to bottom, and a first gap is reserved between the multiple groups of high-frequency coils and the outer magnetic shielding case.
A second gap is left between the high-frequency coil and the inner wall surface of the bell jar.
Furthermore, the distance between two adjacent groups of high-frequency coils is 5-30 mm.
And/or the high-frequency coil is a hollow tube, the outer diameter of the high-frequency coil is 10-30 mm, and the inner diameter of the high-frequency coil is 5-20 mm.
And/or the value of the first gap is 5-50 mm.
And/or the value of the second gap is 10-50 mm.
Furthermore, the inner magnetic shielding case and the outer magnetic shielding case both comprise a straight cylinder section, an upper end enclosure and a lower end enclosure, the upper end enclosure is detachably connected with an upper opening of the straight cylinder section, and the lower end enclosure is detachably connected with a lower opening of the straight cylinder section; the outer magnetic shielding cover is coated on the outer side of the inner magnetic shielding cover and used for surrounding the inner magnetic shielding cover and the inner magnetic shielding cover to form the cavity.
Furthermore, the wall thickness of the inner magnetic shielding case and the wall thickness of the outer magnetic shielding case are both 5-20 mm.
And/or the distance between the inner magnetic shielding case and the outer magnetic shielding case is 10-50 mm.
And/or the inner magnetic shielding case and the outer magnetic shielding case are both made of nickel alloy or low-carbon steel.
Has the advantages that:
according to the treatment device for the inner wall of the reduction furnace, the bell jar can be driven to rotate through the rotating mechanism, and the bell jar and the cold gas power spray gun can rotate relatively, so that the cold gas power spray gun can spray powder to the inner wall surface of the bell jar in the circumferential direction during the rotation process of the bell jar; before that, because the inner wall processing device of the reducing furnace is provided with the high-frequency coil, the high-frequency coil can heat the inner wall surface of the bell jar and heat the inner wall surface of the bell jar to a preset temperature range; because the inner wall surface property of the bell jar is one of the factors influencing the critical speed (the critical speed is a key index in the gas dynamic spraying technology, and the coating can be formed only when the speed of the powder is equal to or greater than the critical speed); or, under the fixed spraying condition, the temperature of the inner wall surface of the bell jar reaches the preset temperature range, so that the mechanical engagement and elastic deformation action of the spraying powder and the inner wall surface of the bell jar are strong, and a coating with higher bonding strength is formed.
According to the foregoing, the inner wall treatment device for the reduction furnace can be used for coating with high bonding strength on the premise of reducing the spraying conditions; alternatively, under fixed spray conditions, a coating with higher bond strength is formed.
In a second aspect, an embodiment of the present invention provides a spraying method for a reduction furnace inner wall treatment apparatus, including the steps of:
the bell jar rotates at a preset speed;
the high-frequency coil generates magnetic induction lines, the magnetic induction lines act on the inner wall surface of the bell jar and generate an eddy current heating effect on the inner wall surface of the bell jar, so that the temperature of the inner wall surface of the bell jar is kept at 50-350 ℃;
spraying powder moving at a high speed by using a cold gas power spray gun, wherein the powder impacts the inner wall surface of a bell jar with the temperature of 50-350 ℃ in a solid state under the supersonic speed state and forms a deposition coating;
and carrying out heat treatment on the deposited coating to form a compact coating.
Preferably, the rotation speed of the bell jar is 0.1-30 rpm.
Preferably, the distance between the spraying port of the cold gas power spray gun and the inner wall surface of the bell jar is 10-50 mm.
Preferably, the cold gas-powered lance is located at an ambient temperature of less than 100 ℃.
Preferably, the temperature for heat treatment of the deposition coating is 300-500 ℃, and the heating time is 10-20 h.
Further, the method also comprises the step of introducing a cooling medium into the high-frequency coil; preferably, the flow rate of the introduced cooling medium is 10-50L/min, and the temperature is 10-30 ℃.
The technical advantages and effects achieved by the spraying method for the inner wall treatment device of the reduction furnace provided by the invention are the same as those achieved by the inner wall treatment device of the reduction furnace, and are not repeated herein.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic structural diagram of a reduction furnace bell jar according to an embodiment of the present invention;
FIG. 2 is a schematic view of the connection among the heating device, the cooling assembly and the cold gas powered spray gun.
Icon:
100-bell jar;
200-a magnetic induction heating assembly; 210-a high frequency coil;
300-a cold gas powered spray gun; 310-a gun body; 320-a spray section;
400-a magnetic shield assembly; 410-an internal magnetic shield; 420-external magnetic shielding case; 430-cooling tube.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or the orientations or positional relationships that the products of the present invention are conventionally placed in use, and are only used for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the devices or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
Furthermore, the terms "horizontal", "vertical" and the like do not imply that the components are required to be absolutely horizontal or pendant, but rather may be slightly inclined. For example, "horizontal" merely means that the direction is more horizontal than "vertical" and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.
In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Some embodiments of the invention are described in detail below with reference to the accompanying drawings. The embodiments described below and the features of the embodiments can be combined with each other without conflict.
The present embodiment provides a device for treating an inner wall of a reduction furnace, as shown in fig. 1 and 2, the device for treating an inner wall of a reduction furnace comprises a bell jar 100, a rotating mechanism (not shown in the drawings), a magnetic induction heating assembly 200, and a cold gas powered lance 300; the bell jar 100 has a closed accommodating space; the rotating mechanism is in transmission connection with the bell jar 100 and is used for driving the bell jar 100 to rotate; the magnetic induction heating assembly 200 comprises a high-frequency coil 210, wherein the high-frequency coil 210 is arranged in the accommodating space and is used for heating the inner wall surface of the bell jar to a preset temperature range (for example, 50-350 ℃); the cold gas powered spray gun 300 is disposed in the accommodating space, and rotates relative to the bell jar 100, for spraying powder to the inner wall surface of the bell jar.
According to the treatment device for the inner wall of the reduction furnace, the bell jar 100 can be driven to rotate through the rotating mechanism, and the bell jar 100 and the cold gas power spray gun 300 can rotate relatively, so that the cold gas power spray gun 300 can spray powder to the inner wall surface of the bell jar in the circumferential direction in the rotating process of the bell jar 100; heretofore, since the reducing furnace inner wall treatment apparatus is provided with the high-frequency coil 210, the high-frequency coil 210 can heat the bell jar inner wall surface and heat the bell jar inner wall surface to a predetermined temperature range; because the inner wall surface property of the bell jar is one of the factors influencing the critical speed (the critical speed is a key index in the gas dynamic spraying technology, and the coating can be formed only when the speed of the powder is equal to or greater than the critical speed); or, under the fixed spraying condition, the temperature of the inner wall surface of the bell jar reaches the preset temperature range, so that the mechanical engagement and elastic deformation action of the spraying powder and the inner wall surface of the bell jar are strong, and a coating with higher bonding strength is formed.
Specifically, the rotating mechanism may be disposed inside the bell jar 100, or outside the bell jar 100; the rotation mechanism for driving the bell jar 100 to rotate is well known in the art, and the present embodiment does not modify the rotation mechanism, and is not described herein. Similarly, the specific structure of the cold gas-powered lance 300 is well known to those skilled in the art, and is not modified in this embodiment, and will not be described herein.
The high-frequency coil 210 is started by power supply control, and after the power supply is turned on, the high-frequency coil 210 is operated, and after the power supply is turned off, the high-frequency coil 210 is stopped.
Further, the inner wall processing device of the reduction furnace further comprises a magnetic shielding assembly 400; the magnetic shield assembly 400 includes a magnetic shield for absorbing an electromagnetic field generated from the high-frequency coil, the magnetic shield being located in the accommodating space; the high-frequency coil 210 is located between the outer peripheral sides of the bell jar and the magnetic shield; the cold gas-powered spray gun 300 includes a gun body portion 310 and a spray portion 320, the gun body portion 310 being located inside a magnetic shield, the spray portion extending out from the magnetic shield and being disposed toward an inner wall surface of a bell jar.
In this embodiment, the high-frequency coil 210 is a hollow tubular structure, and one end of the hollow tubular structure is used for connecting a first liquid inlet pipeline (not shown in the figure) and the other end of the hollow tubular structure is used for connecting a first liquid outlet pipeline (not shown in the figure).
Specifically, the magnetic shield includes an inner magnetic shield 410 and an outer magnetic shield 420, and the inner magnetic shield 410 and the outer magnetic shield 420 enclose a cavity; a cooling pipe 430 is arranged in the cavity, one end of the cooling pipe 430 is used for connecting a second liquid inlet pipeline, and the other end of the cooling pipe 430 is used for connecting a second liquid outlet pipeline.
Optionally, the outer diameter of the cooling tube 430 is 5 to 30mm, for example, 5mm, 10mm, 20mm, 25mm, 30mm, and the like. The inner diameter of the cooling pipe 430 is 2 to 20mm, and may be, for example, 2mm, 5mm, 10mm, 15mm, 20mm, or the like.
As a variation, the cavity has an inlet for connecting to the second liquid inlet line and an outlet for connecting to the second liquid outlet line;
the first liquid inlet pipeline and the second liquid inlet pipeline can be the same pipeline or different pipelines; the first liquid outlet pipeline and the second liquid outlet pipeline can be the same pipeline or different pipelines.
Optionally, the high frequency coil 210, the cooling tube 430 or the cavity may be filled with a cooling fluid, such as water, for heat exchange with the high frequency coil 210 and the magnetic shield, respectively.
Specifically, in this embodiment, the high-frequency coil 210 is a hollow tubular structure, and a cooling liquid is introduced into the tube, because joule heat is generated after the high-frequency coil 210 is energized, and in addition, the high-frequency coil 210 can act on an electromagnetic field to generate eddy currents on the surface, which causes the eddy currents to generate heat, and the heat can be taken away by the cooling liquid to cool the high-frequency coil 210, thereby ensuring the structural strength of the high-frequency coil 210. Similarly, the magnetic shield also can produce the vortex with the electromagnetic field effect, leads to the vortex to generate heat, can take away this part heat through the coolant liquid, and the structural strength of cooling magnetic shield guarantees. Further, since the gun body 310 is provided in the magnetic shield, the magnetic shield can eliminate or absorb the electromagnetic field, and the gun body 310 can be prevented from being adversely affected by the electromagnetic field.
As shown in fig. 1, the high-frequency coils 210 are multiple sets, and the multiple sets of high-frequency coils 210 are sequentially and fixedly wound on the outer periphery of the outer magnetic shielding case 420 from top to bottom, and a first gap is left between the multiple sets of high-frequency coils 210 and the outer magnetic shielding case 420; a second gap is left between the high-frequency coil 210 and the inner wall surface of the bell jar.
In order to facilitate the fixing of the high-frequency coil 210, in the present embodiment, a plurality of coil supports (not shown in the drawings) are disposed on the outer wall of the outer magnetic shielding case 420; each set of coil supports is disposed in correspondence with a set of high frequency coils 210. Optionally, the group of high-frequency coils 210 may be supported and fixed by 3-10 coil supports.
Specifically, the distance between two adjacent sets of high-frequency coils 210 is 5-30 mm, for example, 5mm, 10mm, 20mm, 25mm, 30mm, etc.
Optionally, the high-frequency coil 210 is a hollow tube, and the outer diameter of the high-frequency coil 210 is 10-30 mm, for example, 10mm, 20mm, 25mm, 30mm, or the like; the inner diameter of the high-frequency coil 210 is 5 to 20mm, and may be, for example, 5mm, 10mm, or 20 mm. The high-frequency coil 210 may be made of copper.
Optionally, the value of the first gap is 5-50 mm, for example, 5mm, 10mm, 20mm, 30mm, 40mm, 50mm, and the like.
Optionally, the value of the second gap is 10-50 mm, for example, 10mm, 20mm, 30mm, 40mm, 50mm, and the like.
As shown in fig. 1, the inner magnetic shielding case 410 and the outer magnetic shielding case 420 both include a straight cylinder section, an upper head detachably connected to an upper opening of the straight cylinder section, and a lower head detachably connected to a lower opening of the straight cylinder section; the outer magnetic shield 420 is wrapped outside the inner magnetic shield 410 to enclose a cavity therebetween.
Specifically, the straight cylinder section is composed of at least 2 straight cylinder sections, namely the straight cylinder section can be split into at least two straight cylinder sections. The straight cylinder section and the lower end enclosure comprise avoidance openings with the distance of 100-150 mm (for example, 100mm, 120mm, 140mm, 150mm and the like). The distance between the straight cylinder and the lower end socket and the inner wall of the bell jar 100 is 25 to 130mm, for example, 25mm, 50mm, 75mm, 130mm, etc., preferably, the distance is 25 to 50mm, for example, 25mm, 30mm, 35mm, 40mm, 45mm, 50mm, etc.
Illustratively, the outer magnetic shield 420 and the inner magnetic shield 410 are fixed by a fixing frame, and the fixing frame is fixedly connected to the upper end socket. Optionally, the fixing frame is composed of at least three connecting rods and two circular flat plates, wherein the distance between the connecting rods is at least 500mm, further, the connecting rods are connected with the circular flat plates, one of the circular flat plates is connected with the upper end enclosure through a bolt, and the other circular flat plate is connected with the bell jar 100.
Specifically, the wall thickness of the inner magnetic shield 410 and the wall thickness of the outer magnetic shield 420 are both 5-20 mm, and may be, for example, 5mm, 10mm, 15mm, 20mm, and the like. Optionally, the distance between the inner magnetic shield 410 and the outer magnetic shield 420 is 10-50 mm, for example, 10mm, 20mm, 30mm, 40mm, 50mm, and the like. Optionally, the inner magnetic shielding case 410 and the outer magnetic shielding case 420 are both made of nickel alloy or mild steel.
The embodiment also provides a spraying method of the treatment device for the inner wall of the reduction furnace, which comprises the following steps:
the bell jar 100 rotates at a preset speed;
the high-frequency coil 210 generates magnetic induction lines which act on the inner wall surface of the bell jar and generate an eddy current heating effect on the inner wall surface of the bell jar, so that the temperature of the inner wall surface of the bell jar is kept at 50-350 ℃;
spraying powder moving at high speed by using the cold gas power spray gun 300, wherein the powder impacts the inner wall surface of a bell jar with the temperature of 50-350 ℃ in a solid state under the supersonic speed state, and forms a deposited coating;
carrying out heat treatment on the deposited coating to form a compact coating;
alternatively, the rotation speed of the bell jar 100 is 0.1 to 30rpm, and may be, for example, 0.1rpm, 10rpm, 20rpm, 30rpm, or the like. The distance between the discharge port of the cold gas dynamic spray gun 300 and the inner wall surface of the bell jar is 10 to 50mm, and may be, for example, 10mm, 20mm, 30mm, 40mm, 50mm, or the like. The temperature for heat treatment of the deposited coating is 300 to 500 ℃, and may be, for example, 300 ℃, 400 ℃, 500 ℃ or the like. The heating time is 10 to 20 hours, for example, 10 hours, 15 hours, 20 hours, etc.
In this embodiment, the inner wall of the bell jar 100 is made of one or more of stainless steel, nickel, copper, chromium, titanium, iron, gold, and silver. Preferably, the invention can prepare functional coating on the inner wall of the newly manufactured reduction furnace bell jar, and can repair or thicken the existing coating on the inner wall.
The spraying method of the reducing furnace inner wall treatment device also comprises the step of introducing a cooling medium into the high-frequency coil; preferably, the flow rate of the cooling medium is 10 to 50L/min, for example, 10L/min, or the like. The temperature is 10 to 30 ℃, for example, 10 ℃, 20 ℃, 30 ℃ or the like.
The present invention will be further described with reference to specific examples and comparative examples.
Example 1
The present embodiment provides a device for treating the inner wall of a reduction furnace, as shown in fig. 1, the device for treating the inner wall of a reduction furnace comprises a bell jar 100, a rotating mechanism (not shown in the drawings), a magnetic induction heating assembly 200 and a cold gas powered lance 300; the bell jar 100 has a closed accommodating space; the rotating mechanism is in driving connection with the bell jar 100 and is used for driving the bell jar 100 to rotate.
The magnetic induction heating assembly 200 comprises seven groups of high-frequency coils 210, wherein the seven groups of high-frequency coils 210 are fixedly wound on the outer periphery side of the outer magnetic shielding case 420 from top to bottom in sequence, and a first gap is reserved between the seven groups of high-frequency coils 210 and the outer magnetic shielding case 420; a second gap is left between the high-frequency coil 210 and the inner wall surface of the bell jar.
The high-frequency coil 210 is a hollow tube, and cooling water is introduced into the hollow tube to cool the high-frequency coil 210.
The magnetic shielding case comprises an inner magnetic shielding case 410 and an outer magnetic shielding case 420, wherein a cavity is defined by the inner magnetic shielding case 410 and the outer magnetic shielding case 420; the cavity is internally provided with a cooling pipe 430, and cooling water is introduced into the cooling pipe 430 and used for cooling the inner magnetic shielding case 410 and the outer magnetic shielding case 420.
Referring to fig. 2, the cross-sectional shapes of the inner magnetic shield 410 and the outer magnetic shield 420 are both circular. With continued reference to fig. 2, in order to facilitate the arrangement of the injection portion 320 of the cold gas-powered spray gun 300, the inner magnetic shield 410 and the outer magnetic shield 420 are both provided with an escape opening for the injection portion 320 to pass through, so that the injection portion 320 faces the inner wall surface of the bell jar.
In actual use, the cold gas-powered lance 300 is also coupled with a movement mechanism for driving its movement in the axial direction of the bell jar 100. The cold gas power spray gun 300 is driven to move by the moving mechanism, and the bell jar 100 is driven to rotate by the rotating mechanism, so that the whole spraying of the inner wall surface of the bell jar can be realized. The moving mechanism can be implemented by the prior art and is not described in detail herein.
Example 2
The embodiment provides a spraying method of a treatment device for the inner wall of a reduction furnace, which specifically comprises the following steps:
preheating: rotating the bell jar 100 at a uniform speed around the axis at a speed of 12 rpm;
cooling water of 30L/min and 30 ℃ is introduced into the cooling pipe 430; when the power supply is started, the high-frequency coil 210 starts to generate magnetic induction lines, the inner wall of the bell jar 100 acts on the magnetic induction lines, and an eddy current heating effect is generated on the inner wall surface of the bell jar 100, so that the temperature of the inner wall surface of the bell jar is kept at 50 ℃.
Spraying: the spraying part 320 of the cold gas power spray gun 300 extends out of the escape opening and is opposite to the inner wall surface of the bell jar, and the distance between the spraying part and the inner wall surface is 50 mm; copper powder is sprayed out of the cold gas power spray gun 300, the copper powder impacts the inner wall surface with the temperature of 50 ℃ in a solid state under the supersonic speed state, and the copper powder and the inner wall surface form a sediment body on the inner wall surface through strong elastic deformation and mechanical engagement; during the operation of the high-frequency coil 210, the inner magnetic shield 410 and the outer magnetic shield 420 can block magnetic induction lines from entering cavities of the high-frequency coil and the outer magnetic shield 420, so that the cold gas dynamic spray gun 300 is not affected by the magnetic induction lines, and the cooling water can absorb heat generated by the outer surfaces of the high-frequency coil 210 and the outer magnetic shield 420, so that the ambient temperature of the cold gas dynamic spray gun 300 is lower than 100 ℃.
A heat treatment step: after the completion of the spraying, the coating and the inner wall surface were heated by the high-frequency coil 210 at a temperature of 300 ℃ for 15 hours. Through the heat treatment, mass exchange between the inside of the coating and the inner wall surface of the bell jar 100 can be promoted, the bonding strength of the coating can be promoted, the porosity can be reduced, and the application performance of the coating can be improved.
It should be noted that the above spraying is spraying at a certain height position of the inner wall surface of the bell jar, after the spraying at the certain height position is finished, the moving mechanism is required to drive the cold gas power spray gun 300 to move upwards or downwards so as to spray at another height position of the inner wall surface of the bell jar, and so on.
Example 3
The embodiment provides a spraying method of a treatment device for the inner wall of a reduction furnace, which is different from the embodiment 2 in that: in the preheating step, the temperature of the inner wall surface of the bell jar is maintained at 100 ℃.
Example 4
The embodiment provides a spraying method of a treatment device for the inner wall of a reduction furnace, which is different from the embodiment 2 in that: in the preheating step, the temperature of the inner wall surface of the bell jar was maintained at 200 ℃.
Example 5
The embodiment provides a spraying method of a treatment device for the inner wall of a reduction furnace, which is different from the embodiment 2 in that: in the preheating step, the temperature of the inner wall surface of the bell jar was maintained at 250 ℃.
Example 6
The embodiment provides a spraying method of a treatment device for the inner wall of a reduction furnace, which is different from the embodiment 2 in that: in the preheating step, the inner wall surface temperature of the bell jar was maintained at 300 ℃.
Example 7
The embodiment provides a spraying method of a treatment device for the inner wall of a reduction furnace, which is different from the embodiment 2 in that: in the preheating step, the temperature of the inner wall surface of the bell jar was maintained at 350 ℃.
Comparative example 1
The comparative example provides a spraying method of a treatment device for an inner wall of a reduction furnace, which is different from the method of example 2 in that: in the preheating step, the spraying step and the heat treatment step, the temperature of the inner wall of the bell jar 100 is always kept at the normal temperature; a magnetic shielding cover is not required to be arranged; in the preheating step, cooling water is not required to be introduced into the cooling pipe 430.
In order to compare the technical effects achieved by the examples and comparative examples, the following experimental examples were specifically designed.
Experimental example 1
The temperatures of the inner wall surfaces of the bell jar, the spraying temperatures, the spraying pressures and the bonding strengths used in examples 2 to 7 and comparative example 1 were recorded. The detection method of the bonding strength is based on MH/T3027-2013 thermal spray coating bonding strength test, and specific results are shown in Table 1.
TABLE 1
As can be seen from the data in Table 1, under the same spraying pressure and spraying temperature condition, the bonding strength of the coating is gradually enhanced along with the increase of the temperature of the inner wall surface of the bell jar; compared with the heating of the inner wall surface of the bell jar, when the inner wall surface of the bell jar is at normal temperature, higher spraying pressure and spraying temperature are needed to obtain similar coating bonding strength.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A reducing furnace inner wall processing apparatus, characterized by comprising: a bell jar (100), a rotating mechanism, a magnetic induction heating assembly (200) and a cold gas power spray gun (300);
the bell jar (100) is provided with a closed accommodating space;
the rotating mechanism is in transmission connection with the bell jar (100) and is used for driving the bell jar (100) to rotate;
the magnetic induction heating assembly (200) comprises a high-frequency coil (210), and the high-frequency coil (210) is arranged in the accommodating space and used for heating the inner wall surface of the bell jar to a preset temperature range;
the cold gas power spray gun (300) is arranged in the accommodating space, rotates relative to the bell jar (100) and is used for spraying powder to the inner wall surface of the bell jar.
2. The inner wall treatment device of the reduction furnace according to claim 1, wherein the high-frequency coil (210) is a hollow tubular structure, one end of the hollow tubular structure is used for connecting a liquid inlet pipeline, and the other end of the hollow tubular structure is used for connecting a liquid outlet pipeline.
3. The reduction furnace inner wall treatment apparatus according to claim 1, further comprising a magnetic shield assembly (400);
the magnetic shield assembly (400) comprises a magnetic shield for absorbing an electromagnetic field generated by the high-frequency coil (210), and the magnetic shield is positioned in the accommodating space;
the high-frequency coil (210) is located between the bell jar (100) and an outer peripheral side of the magnetic shield;
the cold gas power spray gun (300) comprises a gun body part (310) and a spraying part (320), wherein the gun body part (310) is located in the magnetic shielding cover, and the spraying part (320) penetrates out of the magnetic shielding cover and faces the inner wall surface of the bell jar.
4. The reduction furnace inner wall processing device according to claim 3, wherein the magnetic shielding case comprises an inner magnetic shielding case (410) and an outer magnetic shielding case (420), and the inner magnetic shielding case (410) and the outer magnetic shielding case (420) enclose a cavity;
a cooling pipe (430) is arranged in the cavity, one end of the cooling pipe (430) is used for being connected with a liquid inlet pipeline, and the other end of the cooling pipe (430) is used for being connected with a liquid outlet pipeline; or the cavity is provided with an inlet and an outlet, the inlet is connected with a liquid inlet pipeline, and the outlet is connected with a liquid outlet pipeline;
preferably, the outer diameter of the cooling pipe (430) is 5-30 mm, and the inner diameter of the cooling pipe (430) is 2-20 mm.
5. The inner wall processing device of the reducing furnace according to claim 4, wherein the high-frequency coils (210) are provided in multiple groups, the multiple groups of high-frequency coils (210) are sequentially and fixedly wound on the outer peripheral side of the outer magnetic shielding case (420) from top to bottom, and a first gap is reserved between the high-frequency coils and the outer magnetic shielding case (420);
a second gap is left between the high-frequency coil (210) and the inner wall surface of the bell jar.
6. The inner wall treatment device of the reduction furnace according to claim 5, wherein the distance between two adjacent groups of the high-frequency coils (210) is 5-30 mm;
and/or the high-frequency coil (210) is a hollow tube, the outer diameter of the high-frequency coil (210) is 10-30 mm, and the inner diameter of the high-frequency coil (210) is 5-20 mm;
and/or the value of the first gap is 5-50 mm;
and/or the value of the second gap is 10-50 mm.
7. The inner wall treatment device of the reducing furnace according to claim 4, wherein the inner magnetic shielding case (410) and the outer magnetic shielding case (420) each comprise a straight cylinder section, an upper end enclosure and a lower end enclosure, the upper end enclosure is detachably connected to an upper opening of the straight cylinder section, and the lower end enclosure is detachably connected to a lower opening of the straight cylinder section; the outer magnetic shielding case (420) is wrapped on the outer side of the inner magnetic shielding case (410) and used for enclosing the inner magnetic shielding case and the inner magnetic shielding case to form the cavity.
8. The inner wall treatment device of the reduction furnace according to claim 7, wherein the wall thickness of the inner magnetic shielding case (410) and the wall thickness of the outer magnetic shielding case (420) are both 5-20 mm;
and/or the distance between the inner magnetic shielding case (410) and the outer magnetic shielding case (420) is 10-50 mm;
and/or the inner magnetic shielding case (410) and the outer magnetic shielding case (420) are both made of nickel alloy or low-carbon steel.
9. A spraying method of a treatment device for the inner wall of a reduction furnace is characterized by comprising the following steps:
the bell (100) rotates at a preset speed;
the high-frequency coil (210) generates magnetic induction lines, the magnetic induction lines act on the inner wall surface of the bell jar and generate an eddy current heating effect on the inner wall surface of the bell jar, so that the temperature of the inner wall surface of the bell jar is kept at 50-350 ℃;
spraying powder moving at high speed by using a cold gas power spray gun (300), wherein the powder impacts the inner wall surface of a bell jar with the temperature of 50-350 ℃ in a solid state under a supersonic speed state and forms a deposition coating;
carrying out heat treatment on the deposited coating to form a compact coating;
preferably, the rotation speed of the bell jar (100) is 0.1-30 rpm;
preferably, the distance between the spray port of the cold gas power spray gun (300) and the inner wall surface of the bell jar is 10-50 mm;
preferably, the cold gas powered lance (300) is located in an environment at a temperature of less than 100 ℃;
preferably, the temperature for heat treatment of the deposition coating is 300-500 ℃, and the heating time is 10-20 h.
10. The method for spraying an apparatus for treating an inner wall of a reducing furnace according to claim 9, further comprising a step of introducing a cooling medium into the high-frequency coil (210); preferably, the flow rate of the introduced cooling medium is 10-50L/min, and the temperature is 10-30 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114570288A (en) * | 2021-09-28 | 2022-06-03 | 常州顺钿精密科技有限公司 | Vertical continuous reaction furnace for preparing silicon oxide |
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