A tubular heating device for preparing silicon oxide and a control method thereof

Abstract

The present invention relates to a tubular heating device for preparing silicon oxide, characterized in that it comprises: a furnace frame base is arranged below the tubular heating device for preparing silicon oxide; a furnace chamber is fixed above the furnace frame base; a furnace tube structure is horizontally inserted into the furnace chamber; the furnace tube structure is fixed on the furnace chamber through a flange; a main control system controls the temperature of the furnace tube structure; silicon oxide is prepared in a reaction crucible arranged in the furnace tube structure, and silicon oxide powder is collected in a collection bucket in the furnace tube structure. The present silicon oxide production device is composed of a vacuum-evacuable alumina ceramic refractory tube, and when working, the mixed SiO2 and Si are placed at one end of a sealed tube, heated in a vacuum state until the raw materials are gasified, and then deposited at the other end of the refractory tube. However, this device has technical problems such as low production efficiency and the reaction tube is very easy to break.

Description

Technical Field

[0001] The embodiments of the present invention relate to a tubular heating device and a control method thereof, and in particular to a tubular heating device for producing silicon monoxide and a control method thereof. Background Art

[0002] Silicon oxide powder is extremely active and can be used as a raw material for the synthesis of fine ceramics such as silicon nitride and silicon carbide. It can be evaporated in a vacuum and coated on the metal reflective mirror used in optical instruments to be used as optical glass and semiconductor materials. Silicon oxide can also be used to prepare lithium-ion battery negative electrode materials with excellent performance.

[0003] The principle of preparing silicon oxide is Si+SiO2→SiO, silicon powder and silicon dioxide are mixed in a 1:1 molar ratio, and the product is obtained after heating under vacuum conditions. This reaction is a reversible reaction. If the pressure is further reduced and the temperature is increased, the equilibrium will move to the silicon oxide side.

[0004] At present, the silicon oxide production device is composed of a vacuum-evacuable alumina ceramic refractory tube. When working, the mixed SiO2 and Si are placed at one end of the sealed tube, heated under vacuum until the raw materials are gasified, and then deposited at the other end of the refractory tube. However, this device has the disadvantages of low production efficiency and the reaction tube is very easy to break. Summary of the invention

[0005] The purpose of the embodiments of the present invention is to provide a tubular heating device for preparing silicon 2 oxide with high efficiency and a control method thereof.

[0006] In order to achieve the above object, the embodiment of the present invention designs a tubular heating device for preparing silicon dioxide, comprising:

[0007] A furnace base, wherein the furnace base is arranged below the horizontal vacuum tube furnace;

[0008] A furnace, the furnace being fixed above the furnace frame base;

[0009] A furnace tube structure is inserted transversely into the furnace; the furnace tube structure is fixed to the furnace through a flange;

[0010] A main control system controls the temperature of the furnace tube structure; prepares silicon oxide in a reaction crucible arranged in the furnace tube structure, and collects silicon oxide powder in a collection bucket in the furnace tube structure.

[0011] Furthermore, the furnace frame base further comprises:

[0012] A furnace frame is arranged in the middle of the furnace frame base and below the furnace chamber; the furnace frame is constructed of a plurality of square tubes to form a square structure;

[0013] A front side plate, fixed to the front side of the furnace frame;

[0014] Side panels are fixed on the left and right sides of the furnace frame;

[0015] A rear side plate, fixed to the rear side of the furnace frame; a plurality of rows and columns of heat dissipation holes are provided on the rear side plate;

[0016] A slide is above the furnace frame and fixed on both sides of the furnace.

[0017] Furthermore, the furnace further comprises:

[0018] An upper furnace structure, wherein the upper furnace structure is arranged above the furnace;

[0019] A lower furnace structure, which is arranged below the upper furnace structure;

[0020] The upper furnace structure is connected to the lower furnace structure via a hinge arranged on one side, so that the upper furnace structure is flipped to one side;

[0021] A through hole is transversely opened on the lower furnace structure; the furnace tube structure is transversely inserted into the through hole; and the furnace tube structure is fixed to both sides of the lower furnace structure through flanges at both ends.

[0022] Furthermore, the upper furnace structure further comprises:

[0023] An upper furnace frame is arranged on the inner side of the upper furnace structure;

[0024] An upper furnace body top cover plate, the upper furnace body top cover plate being fixed on one side above the upper furnace frame;

[0025] Upper furnace body side cover plates, fixed on both sides of the upper furnace frame;

[0026] An upper furnace cover plate, fixed to the front and rear of the upper furnace frame;

[0027] A furnace installation box is fixed on the inner side of the upper furnace frame;

[0028] A furnace, wherein the furnace is fixed to the furnace installation box by bolts above the furnace, so that the furnace and the furnace installation box are connected as one;

[0029] A silicon carbon rod is fixed from top to bottom on the inner side of the furnace and one side of the furnace installation box.

[0030] Furthermore, the lower furnace structure further includes:

[0031] A lower furnace frame is arranged on the inner side of the lower furnace structure;

[0032] A pressing plate, fixed above the lower furnace frame;

[0033] A decorative plate, fixed on the top of the pressing plate;

[0034] A left cover plate of the furnace body, a middle plate of the furnace body and a right cover plate of the furnace body are fixed in sequence on one side of the lower furnace frame;

[0035] A furnace body side middle plate, the furnace body side middle plate is fixed on one side of the lower furnace frame; the through hole is opened on the furnace body side middle plate; the furnace tube structure is horizontally inserted into the through hole;

[0036] A furnace body side plate, on one side of the furnace body side middle plate, fixed to the lower furnace frame;

[0037] An outer furnace shell is fixed on the inner side of the lower furnace frame;

[0038] An inner furnace shell is arranged on the inner side of the outer furnace shell, and a silicon carbon rod is inserted between the outer furnace shell and the inner furnace shell;

[0039] Insulation side plates are fixed on both sides of the inner furnace shell and the outer furnace shell; the through holes are also provided on the insulation side plates;

[0040] A heat-insulating front plate, fixed inside the other side of the lower furnace frame;

[0041] Insulation baffle; the insulation baffle is arranged between the insulation front plate and the inner furnace shell; the through hole is also opened on the insulation baffle.

[0042] Furthermore, the furnace tube structure further comprises:

[0043] Flange end cover plates are arranged at both ends of the furnace tube structure, and the flange end cover plates and the clamping flange form a quick-release structure through an upper hinge seat; notches are provided on the flange end cover plates and the clamping flange, and fixing bolts are arranged in the notches for fixing the flange end cover plates and the clamping flange;

[0044] A vacuum tube is provided on the furnace tube between the flange end cover plate and the clamping flange; the vacuum tube is connected to the furnace tube;

[0045] A protective gas injection pipe is fixed on the furnace tube between the flange end cover plate and the clamping flange; the protective gas injection pipe is connected to the furnace tube;

[0046] A fixing flange is fixed on the outer side of the furnace tube between the clamping flanges; the fixing flange is fixed to the side middle plate of the furnace body by bolts.

[0047] Furthermore, the furnace tube further comprises:

[0048] A pipe plug is inserted into one end of the furnace tube in the furnace tube;

[0049] A reaction crucible is arranged in the furnace tube on one side of the tube plug;

[0050] A material receiving barrel is arranged at the other end of the furnace tube;

[0051] A gradient brick is arranged between the reaction crucible and the material receiving barrel.

[0052] Furthermore, the main control system further includes:

[0053] A main control device, which is arranged in the main control system and is electrically connected to a temperature controller, a vacuum gauge, and a vacuum pump control device;

[0054] The temperature controller controls the silicon carbon rod to heat;

[0055] The vacuum gauge controls the vacuum degree of the furnace tube;

[0056] The vacuum pump control device controls the start and stop of the vacuum pump.

[0057] The present invention also provides a control method for a tubular heating device for preparing silicon dioxide, which further comprises the following steps:

[0058] Step S10, placing the sample: placing the sample in the reaction crucible, pushing it into the furnace tube, and plugging it into the tube; closing the flange end cover plate, sealing the flange end cover plate and the furnace tube, and entering step S20;

[0059] Step S20: Setting parameters: Setting the heating temperature in the furnace tube, the vacuum degree of the furnace tube and the reaction time in the main control system; proceeding to step S30;

[0060] Step S30: extracting vacuum: the main control device controls the vacuum pump control device to start the vacuum pump to evacuate the furnace; then proceed to step S40;

[0061] Step S40: Determine the vacuum value: the main control device reads the data of the vacuum gauge. If the data of the vacuum gauge is lower than the preset vacuum degree, the process proceeds to step S50; if the data of the vacuum gauge is higher than the preset vacuum degree, the process proceeds to step S60;

[0062] Step S50: vacuum control, the vacuum pump stops extracting vacuum to ensure that the vacuum degree in the furnace tube is within the preset vacuum degree deviation range. If the vacuum degree is higher than the preset vacuum degree deviation range, the main control device controls the vacuum pump to extract vacuum; if the vacuum degree is lower than the preset vacuum degree deviation range, the vacuum pump stops working; and proceed to step S70;

[0063] Step S60: Check whether the horizontal vacuum tube furnace is leaking, and repeat step S10;

[0064] Step S70: Heating: the main control device controls the output of the temperature controller to control the silicon carbon rod to heat; then proceed to step S80;

[0065] Step S80: Determine the temperature: The temperature controller determines whether the preset temperature has been reached. If the preset temperature has been reached, the process proceeds to step S90; if the preset temperature has not been reached, the process repeats step S70 in a loop.

[0066] Step S90: Keep warm: the main control device controls the output of the temperature controller to control the silicon carbon rod to keep warm until the preset reaction time returns to zero; then proceed to step S100;

[0067] Step S100: taking materials: the main control device controls the temperature controller to stop output, and after the heating program is completed, the material receiving barrel is taken out, and after cooling, the vacuum of the furnace tube is broken; the flange end cover is opened; and the required silicon oxide is obtained on the barrel wall of the material receiving barrel.

[0068] The main control device in the control method of the tubular heating equipment for preparing silicon 2 oxide further controls the temperature controller to control the furnace tube heating using PID control.

[0069] Compared with the prior art, the embodiment of the present invention adopts a tubular heating device for preparing silicon dioxide, which has the characteristics of high efficiency in preparing silicon dioxide. At the same time, a structure in which a furnace tube structure is horizontally inserted into the furnace and the furnace tube structure is fixed on the furnace through a flange is adopted, and two temperature zones are set, and a thermal insulation material is used as a partition to form a clear temperature gradient. The high temperature zone is the reaction zone, and the low temperature zone is the collection zone, and the production efficiency has been significantly improved compared with the current products. The thermal insulation structure is optimized, the energy utilization rate is improved, and the temperature during the actual reaction is higher, and the production efficiency is improved, which can well realize the characteristics of simple structure and convenient feeding and taking materials; it solves the problem that the current silicon dioxide production device is composed of a vacuum-evacuable alumina ceramic refractory tube, and the mixed SiO2 and Si are placed at one end of the sealed tube during operation, and heated under a vacuum state until the raw materials are gasified, and then deposited at the other end of the refractory tube. However, this device has technical problems such as low production efficiency and the reaction tube is very easy to break. BRIEF DESCRIPTION OF THE DRAWINGS

[0070] Figure 1 It is a schematic diagram of the three-dimensional structure of the present invention;

[0071] Figure 2 It is a schematic diagram of the upper furnace structure of the present invention;

[0072] Figure 3 It is a schematic diagram of the lower furnace structure of the present invention;

[0073] Figure 4 A schematic diagram of a furnace base of the present invention;

[0074] Figure 5 It is a schematic diagram of the furnace tube structure of the present invention;

[0075] Figure 6 It is a schematic diagram of the furnace tube structure in the cutting direction of the present invention;

[0076] Figure 7 It is a control schematic diagram of the main control system of the present invention;

[0077] Figure 8 It is a flow chart of the control method of the present invention. DETAILED DESCRIPTION

[0078] In order to make the purpose, technical scheme and advantages of the present invention clearer, the following will be described in detail with reference to the accompanying drawings. However, it will be appreciated by those skilled in the art that in the various embodiments of the present invention, many technical details are provided in order to enable the reader to better understand the present application. However, even without these technical details and various changes and modifications based on the following embodiments, the technical scheme claimed for protection in the claims of the present application can be implemented.

[0079] The first embodiment of the present invention relates to a tubular heating device for preparing silicon oxide, such as Figure 1 , Figure 7 As shown, including:

[0080] A furnace frame base 3 is arranged below the tubular heating device for preparing silicon oxide in the present embodiment; the furnace frame base 3 is mainly used to support the tubular heating device for preparing silicon oxide in the present embodiment.

[0081] A furnace 1 is fixed above the furnace frame base 3; the furnace 1 plays a heating role in this embodiment.

[0082] The furnace tube structure 2 is inserted horizontally into the furnace 1; the furnace tube structure 2 is fixed to the furnace 1 through a flange; the furnace tube structure 2 is mainly used for preparing silicon oxide in the tubular heating equipment for preparing silicon oxide in this embodiment, and is the core component in this embodiment.

[0083] A main control system controls the temperature of the furnace tube structure; prepares silicon oxide in a reaction crucible arranged in the furnace tube structure, and collects silicon oxide powder in a collection bucket in the furnace tube structure.

[0084] In this embodiment, the tubular heating equipment used to prepare silicon iodine has the characteristics of high efficiency in preparing silicon iodine. At the same time, a structure in which a furnace tube structure is horizontally inserted into the furnace and fixed to the furnace through a flange is adopted, and two temperature zones are set, and a thermal insulation material is used as a partition to form a clear temperature gradient. The high temperature zone is the reaction zone, and the low temperature zone is the collection zone. The production efficiency has been significantly improved compared with the current products. The thermal insulation structure is optimized, the energy utilization rate is improved, and the temperature during the actual reaction is higher, and the production efficiency is improved, which can well realize the characteristics of simple structure, convenient feeding and taking materials; it solves the problem that the current silicon iodine production device is composed of a vacuum-evacuable alumina ceramic refractory tube. When working, the mixed SiO2 and Si are placed at one end of the sealed tube, heated in a vacuum state until the raw materials are gasified, and then deposited at the other end of the refractory tube. However, this device has technical problems such as low production efficiency and the reaction tube is very easy to break.

[0085] In order to achieve the above technical effects, Figure 4 As shown, the furnace frame base 3 also includes:

[0086] A furnace frame 3-1 is provided in the middle of the furnace frame base 3 and below the furnace 1; the furnace frame 3-1 is constructed of a plurality of square tubes to form a square structure;

[0087] A front side plate 3-2 is fixed on the front side of the furnace frame 3-1;

[0088] Fix the side panels 3-3 on the left and right sides of the furnace frame 3-1;

[0089] A rear side plate 3-4 is fixed to the rear side of the grate 3-1; a plurality of rows and columns of heat dissipation holes 3-5 are provided on the rear side plate 3-4; the front side plate 3-2, the side plate 3-3, the rear side plate 3-4 and the grate 3-1 constitute the structure of the grate base 3.

[0090] Above the furnace frame 3-1, slides 4 are fixed on both sides of the furnace 1. The slides 4 are used to place the reaction crucible 2-5-2 and the collection bucket 2-5-4.

[0091] In order to achieve the above technical effects, Figure 1 , Figure 2 , Figure 3 As shown, the furnace 1 also includes:

[0092] The upper furnace structure 11 is arranged above the furnace 1;

[0093] A lower furnace structure 12 is arranged below the upper furnace structure 11;

[0094] The upper furnace structure 11 is connected to the lower furnace structure 12 via a hinge 1-20 disposed on one side, so that the upper furnace structure 11 is flipped to one side.

[0095] A through hole 1-21 is horizontally opened on the lower furnace structure 12; the furnace tube structure 2 is horizontally inserted into the through hole 1-21; the furnace tube structure 2 is fixed to both sides of the lower furnace structure 12 through flanges at both ends. The upper furnace structure 11 and the lower furnace structure 12 are connected by hinges 1-20 to form a flip structure. At the same time, a through hole 1-21 is horizontally opened on the lower furnace structure 12 for installing the furnace tube structure 2.

[0096] In order to achieve the above technical effects, Figure 2 As shown, the upper furnace structure 11 further includes:

[0097] An upper furnace frame 1-18 is arranged inside the upper furnace structure 11; the upper furnace frame 1-18 serves as a frame structure of the upper furnace structure 11;

[0098] An upper furnace body top cover plate 1-13 is fixed on one side above the upper furnace frame 1-18;

[0099] The upper furnace body side cover plates 1-14 are fixed on both sides of the upper furnace frame 1-18;

[0100] The upper furnace cover plate 1-15 is fixed at the front and rear of the upper furnace frame 1-18;

[0101] A furnace installation box 1-16 is fixed on the inner side of the upper furnace frame 1-18;

[0102] The upper furnace body top cover plate 1-13, the upper furnace body side cover plate 1-14, and the upper furnace body cover plate 1-15 are arranged around the upper furnace frame 1-18.

[0103] The furnace 1-17 is fixed to the top of the furnace installation box 1-16 by bolts, so that the furnace 1-17 and the furnace installation box 1-16 are connected as a whole;

[0104] A silicon carbon rod 1-19 is fixed from top to bottom on the inner side of the furnace 1-17 and the furnace installation box 1-16. The silicon carbon rod 1-19 is used as a heating component in the furnace installation box 1-16 and the furnace 1-17.

[0105] Similarly, in order to achieve the above technical effects, Figure 3 As shown, the lower furnace structure 12 further includes:

[0106] A lower furnace frame 1-0 is arranged inside the lower furnace structure 12; the lower furnace frame 1-0 is used as a frame structure of the lower furnace structure 12;

[0107] A pressing plate 1-2 is fixed above the lower furnace frame 1-0;

[0108] A decorative plate 1-1 is fixed above the pressing plate 1-2; the pressing plate 1-2 and the decorative plate 1-1 serve as a fixed structure above the lower furnace frame 1-0;

[0109] A left cover plate 1-3, a middle plate 1-4 and a right cover plate 1-5 of the furnace body are fixed in sequence on one side of the lower furnace frame 1-0;

[0110] A furnace body side middle plate 1-6 is fixed on one side of the lower furnace frame 1-0; a through hole 1-21 is opened on the furnace body side middle plate 1-6; and the furnace tube structure 2 is horizontally inserted into the through hole 1-21;

[0111] On one side of the furnace body side middle plate 1-6, a furnace body side plate 1-7 is fixed to the lower furnace frame 1-0; the furnace body side middle plate 1-6 and the furnace body side plate 1-7 constitute a baffle on one side of the lower furnace frame 1-0;

[0112] An outer furnace shell 1-8 is fixed on the inner side of the lower furnace frame 1-0;

[0113] An inner furnace shell 1-9 is arranged inside the outer furnace shell 1-8, and a silicon carbon rod 1-19 is inserted between the outer furnace shell 1-8 and the inner furnace shell 1-9; the outer furnace shell 1-8 and the inner furnace shell 1-9 constitute the furnace shell structure in this embodiment;

[0114] The heat-insulating side plates 1-10 are fixed on both sides of the inner furnace shell 1-9 and the outer furnace shell 1-8; through holes 1-21 are also provided on the heat-insulating side plates 1-10; the heat-insulating side plates 1-10 are used for heat preservation.

[0115] The heat-insulating front plate 1-11 is fixed inside the other side of the lower furnace frame 1-0;

[0116] Insulating baffle 1-12; the insulating baffle 1-12 is arranged between the insulating front plate 1-11 and the inner furnace shell 1-9; similarly, a through hole 1-21 is opened on the insulating baffle 1-12.

[0117] Similarly, in order to achieve the above technical effects, Figure 5 As shown, the furnace tube structure 2 also includes:

[0118] Flange end cover plate 2-1, flange end cover plates 2-1 are arranged at both ends of the furnace tube structure 2, and the flange end cover plate 2-1 and the clamping flange 2-2 form a quick-release structure through an upper hinge seat 2-4; a notch 2-6 is opened on the flange end cover plate 2-1 and the clamping flange 2-2, and fixing bolts are arranged in the notch 2-6 for fixing the flange end cover plate 2-1 and the clamping flange 2-2;

[0119] A vacuum tube 2-7 is arranged on the furnace tube 2-5 between the flange end cover plate 2-1 and the clamping flange 2-2; the vacuum tube 2-7 is connected with the furnace tube 2-5; and the vacuum tube 2-7 is used for extracting vacuum from the furnace tube structure 2.

[0120] A protective gas injection pipe 2-8 is fixed on the furnace tube 2-5 between the flange end cover plate 2-1 and the clamping flange 2-2; the protective gas injection pipe 2-8 is connected to the furnace tube 2-5; the protective gas injection pipe 2-8 is used for injecting protective gas to destroy the vacuum of the furnace tube structure 2 and protect the metal in the furnace tube structure 2.

[0121] Between the clamping flanges 2-2, a fixing flange 2-3 is fixed on the outside of the furnace tube 2-5; the fixing flange 2-3 is bolted to the furnace body side middle plate 1-6. The fixing flange 2-3 is used to fix the furnace tube structure 2. The above-mentioned furnace tube structure 2 is the external structure of the furnace tube structure 2, which is mainly used to install the furnace tube structure 2 on the lower furnace structure 12 to achieve

[0122] Similarly, in order to achieve the above technical effects, Figure 6 As shown, the furnace tube 2-5 also includes:

[0123] In the furnace tube 2-5, a pipe plug 2-5-1 is inserted into one end of the furnace tube 2-5; the pipe plug 2-5-1 is used to isolate the space of metal in the furnace tube 2-5;

[0124] In the furnace tube 2-5, a reaction crucible 2-5-2 is arranged on one side of the tube plug 2-5-1; the reaction crucible 2-5-2 is used to heat the mixed raw materials of SiO2 and Si.

[0125] A material collecting barrel 2-5-4 is provided at the other end of the furnace tube 2-5; the material collecting barrel 2-5-4 is used to collect metal powder;

[0126] A gradient brick 2-5-3 is set between the reaction crucible 2-5-2 and the receiving barrel 2-5-4. The gradient brick 2-5-3 is mainly used to block metal vapor. When the metal vapor passes over the gradient brick 2-5-3, since the gradient brick 2-5-3 is stepped, the metal vapor will be cooled quickly and metal powder will be formed quickly. In this way, the gradient brick 2-5-3 can better obtain metal powder.

[0127] In order to achieve the above technical effects, Figure 7 As shown, the main control system 8 also includes:

[0128] A main control device 8-1 is provided in the main control system 8, and the main control device 8-1 is electrically connected to the temperature controller 8-2, the vacuum gauge 8-3, and the vacuum pump control device 8-4; in the main control system 8 of this embodiment, the main control device 8-1 is provided to control the temperature controller 8-2, the vacuum gauge 8-3, the vacuum pump control device 8-4 and other components, so that the silicon carbon rod 1-19 in this embodiment heats the furnace tube 2-5, and the mixed SiO2 and Si in the reaction crucible 2-5-2 react to form silicon dioxide;

[0129] The temperature controller 8-2 controls the silicon carbon rod 1-19 to heat;

[0130] In this embodiment, during the process of extracting vacuum, the vacuum gauge 8-3 controls the vacuum degree of the furnace tube 2-5, and the vacuum pump control device 8-4 controls the start and stop of the vacuum pump 8-5.

[0131] In a second embodiment of the present invention, a control method for a tubular heating device for preparing silicon 2 oxide is also disclosed, which further includes the following steps:

[0132] Step S10, placing the sample: placing the sample in the reaction crucible 2-5-2, pushing it into the furnace tube 2-5, and plugging it into the pipe plug 2-5-1; closing the flange end cover 2-1, sealing the flange end cover 2-1 and the furnace tube 2-5, and entering step S20;

[0133] Step S20: Setting parameters: Setting the heating temperature in the furnace tube 2-5, the vacuum degree of the furnace tube 2-5 and the reaction time in the main control system 8; proceeding to step S30;

[0134] Step S30: extracting vacuum: the main control device 8-1 controls the vacuum pump control device 8-4 to start the vacuum pump 8-5 to evacuate the furnace 1; then proceed to step S40;

[0135] Step S40: Determine the vacuum value: the main control device 8-1 reads the data of the vacuum gauge 8-3. If the data of the vacuum gauge 8-3 is lower than the preset vacuum degree, the process proceeds to step S50; if the data of the vacuum gauge 8-3 is higher than the preset vacuum degree, the process proceeds to step S60;

[0136] Step S50: vacuum control, the vacuum pump 8-5 stops extracting vacuum to ensure that the vacuum degree in the furnace tube 2-5 is within the preset vacuum degree deviation range. If the vacuum degree is higher than the preset vacuum degree deviation range, the main control device 8-1 controls the vacuum pump 8-5 to extract vacuum; if the vacuum degree is lower than the preset vacuum degree deviation range, the vacuum pump 8-5 stops working; enter step S70;

[0137] Step S60: Check whether the horizontal vacuum tube furnace is leaking, and repeat step S10;

[0138] Step S70: Heating: the main control device 8-1 controls the output of the temperature controller 8-2 to control the silicon carbon rod 1-19 to heat; proceed to step S80;

[0139] Step S80: Determine the temperature: The temperature controller 8-2 determines whether the preset temperature has been reached. If the preset temperature has been reached, the process proceeds to step S90; if the preset temperature has not been reached, the process repeats step S70 in a loop;

[0140] Step S90: Keep warm: the main control device 8-1 controls the output of the temperature controller 8-2 to control the silicon carbon rod 1-19 to keep warm until the preset reaction time returns to zero; then proceed to step S100;

[0141] Step S100: taking materials: the main control device 8-1 controls the temperature controller 8-2 to stop output. After the heating program is completed, the material receiving barrel 2-5-4 is taken out. After cooling, the vacuum of the furnace tube 2-5 is broken; the flange end cover plate 2-1 is opened; and the required silicon oxide is obtained on the barrel wall of the material receiving barrel 2-5-4.

[0142] In the control method of the tubular heating equipment for preparing silicon 2 oxide in this embodiment, the main control device 8-1 controls the temperature controller 8-2 to control the heating of the furnace tube 2-5 using PID control.

[0143] Those skilled in the art will appreciate that the above-mentioned embodiments are specific examples for implementing the present invention, and in actual applications, various changes may be made thereto in form and detail without departing from the spirit and scope of the present invention.

Claims

1. A tubular heating device for preparing silicon oxide, characterized in that: include: A furnace base, which is arranged below the tubular heating device for preparing silicon 2 oxide; A furnace, the furnace being fixed above the furnace frame base; A furnace tube structure is inserted transversely into the furnace; the furnace tube structure is fixed to the furnace through a flange; A main control system, wherein the main control system controls the temperature of the furnace tube structure; prepares silicon oxide in a reaction crucible provided in the furnace tube structure, and collects silicon oxide powder in a collection bucket in the furnace tube structure; The furnace frame base further comprises: A furnace frame is arranged in the middle of the furnace frame base and below the furnace chamber; the furnace frame is constructed of a plurality of square tubes to form a square structure; A front side plate, fixed to the front side of the furnace frame; Side panels are fixed on the left and right sides of the furnace frame; A rear side plate, fixed to the rear side of the furnace frame; a plurality of rows and columns of heat dissipation holes are provided on the rear side plate; A slide, above the furnace frame, fixed on both sides of the furnace; The furnace further comprises: An upper furnace structure, wherein the upper furnace structure is arranged above the furnace; A lower furnace structure, which is arranged below the upper furnace structure; The upper furnace structure is connected to the lower furnace structure via a hinge arranged on one side, so that the upper furnace structure is flipped to one side; A through hole is transversely opened on the lower furnace structure; the furnace tube structure is transversely inserted into the through hole; the furnace tube structure is fixed to both sides of the lower furnace structure through flanges at both ends; The upper furnace structure further comprises: An upper furnace frame is arranged on the inner side of the upper furnace structure; An upper furnace body top cover plate, the upper furnace body top cover plate being fixed on one side above the upper furnace frame; Upper furnace body side cover plates, fixed on both sides of the upper furnace frame; An upper furnace cover plate, fixed to the front and rear of the upper furnace frame; A furnace installation box is fixed on the inner side of the upper furnace frame; A furnace, wherein the furnace is fixed to the furnace installation box by bolts above the furnace, so that the furnace and the furnace installation box are connected as one; A silicon carbon rod is fixed from top to bottom on the inner side of the furnace and one side of the furnace installation box; The lower furnace structure further comprises: A lower furnace frame is arranged on the inner side of the lower furnace structure; A pressing plate, fixed above the lower furnace frame; A decorative plate, fixed on the top of the pressing plate; A left cover plate of the furnace body, a middle plate of the furnace body and a right cover plate of the furnace body are fixed in sequence on one side of the lower furnace frame; A furnace body side middle plate, the furnace body side middle plate is fixed on one side of the lower furnace frame; the through hole is opened on the furnace body side middle plate; the furnace tube structure is horizontally inserted into the through hole; A furnace body side plate, on one side of the furnace body side middle plate, fixed to the lower furnace frame; An outer furnace shell is fixed on the inner side of the lower furnace frame; An inner furnace shell is arranged on the inner side of the outer furnace shell, and a silicon carbon rod is inserted between the outer furnace shell and the inner furnace shell; Insulation side plates are fixed on both sides of the inner furnace shell and the outer furnace shell; the through holes are also provided on the insulation side plates; A heat-insulating front plate, fixed inside the other side of the lower furnace frame; Insulation baffle; the insulation baffle is arranged between the insulation front plate and the inner furnace shell; the through hole is also provided on the insulation baffle; The furnace tube structure further comprises: Flange end cover plates are arranged at both ends of the furnace tube structure, and the flange end cover plates and the clamping flange form a quick-release structure through an upper hinge seat; notches are provided on the flange end cover plates and the clamping flange, and fixing bolts are arranged in the notches for fixing the flange end cover plates and the clamping flange; A vacuum tube is provided on the furnace tube between the flange end cover plate and the clamping flange; the vacuum tube is connected to the furnace tube; A protective gas injection pipe is fixed on the furnace tube between the flange end cover plate and the clamping flange; the protective gas injection pipe is connected to the furnace tube; A fixing flange is fixed between the clamping flanges on the outside of the furnace tube; the fixing flange is fixed to the furnace body side middle plate by bolts; The furnace tube further comprises: A pipe plug is inserted into one end of the furnace tube in the furnace tube; A reaction crucible is arranged in the furnace tube on one side of the tube plug; A material receiving barrel is arranged at the other end of the furnace tube; A gradient brick, which is arranged between the reaction crucible and the material receiving barrel; The main control system further includes: A main control device, which is arranged in the main control system and is electrically connected to a temperature controller, a vacuum gauge, and a vacuum pump control device; The temperature controller controls the silicon carbon rod to heat; The vacuum gauge controls the vacuum degree of the furnace tube; The vacuum pump control device controls the start and stop of the vacuum pump.

2. A control method for a tubular heating device for preparing silicon oxide, using the tubular heating device for preparing silicon oxide according to claim 1, characterized in that: The steps include: Step S10, placing the sample: placing the sample in the reaction crucible, pushing it into the furnace tube, and plugging it into the tube; closing the flange end cover plate, sealing the flange end cover plate and the furnace tube, and entering step S20; Step S20: Setting parameters: Setting the heating temperature in the furnace tube, the vacuum degree of the furnace tube and the reaction time in the main control system; proceeding to step S30; Step S30: extracting vacuum: the main control device controls the vacuum pump control device to start the vacuum pump to evacuate the furnace; Go to step S40; Step S40: Determine the vacuum value: the main control device reads the data of the vacuum gauge. If the data of the vacuum gauge is lower than the preset vacuum degree, the process proceeds to step S50; if the data of the vacuum gauge is higher than the preset vacuum degree, the process proceeds to step S60; Step S50: vacuum control, the vacuum pump stops extracting vacuum to ensure that the vacuum degree in the furnace tube is within the preset vacuum degree deviation range. If the vacuum degree is higher than the preset vacuum degree deviation range, the main control device controls the vacuum pump to extract vacuum; if the vacuum degree is lower than the preset vacuum degree deviation range, the vacuum pump stops working; and proceed to step S70; Step S60: Check whether the tubular heating equipment for preparing silicon 2 oxide is leaking, and repeat step S10; Step S70: Heating: the main control device controls the output of the temperature controller to control the silicon carbon rod to heat; then proceed to step S80; Step S80: Determine the temperature: The temperature controller determines whether the preset temperature has been reached. If the preset temperature has been reached, the process proceeds to step S90; if the preset temperature has not been reached, the process repeats step S70 in a loop. Step S90: Keep warm: the main control device controls the output of the temperature controller to control the silicon carbon rod to keep warm until the preset reaction time returns to zero; then proceed to step S100; Step S100: taking materials: the main control device controls the temperature controller to stop output, and after the heating program is completed, the material receiving barrel is taken out, and after cooling, the vacuum of the furnace tube is broken; the flange end cover is opened; and the required silicon oxide is obtained on the barrel wall of the material receiving barrel.

3. The control method of a tubular heating device for preparing silicon oxide according to claim 2, characterized in that: The main control device controls the temperature controller to control the furnace tube heating in a PID control manner.

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