Silicon oxide preparation device

Abstract

A device for preparing silicon oxide includes a heating furnace, a heating device, a crucible, a deposition box, at least one exhaust pipe and an exhaust device, wherein the crucible and the deposition box are arranged in the heating furnace, the heating device heats the crucible so that the solid raw material placed in the crucible forms a gaseous silicon oxide, the deposition box has at least one air inlet and an air outlet, and at least one adsorbent is arranged inside the deposition box; the first end of the at least one exhaust pipe is arranged at a position adjacent to the upper opening of the crucible, and the second end of the at least one exhaust pipe is connected to the at least one air inlet of the deposition box; the exhaust device is connected to the air outlet of the deposition box to extract the gaseous silicon oxide from the crucible and make the gaseous silicon oxide contact with the surface of the at least one adsorbent to deposit a solid silicon oxide.

Description

Technical Field

[0001] The present invention relates to a preparation device for silicon oxide, and in particular to a preparation device capable of increasing the yield of silicon oxide. Background Art

[0002] Known secondary batteries include nickel-cadmium batteries, nickel-metal hydride batteries, lithium-ion secondary batteries, etc. Compared with nickel-cadmium batteries or nickel-metal hydride batteries, lithium-ion secondary batteries have the characteristics of high energy density, high operating voltage, small memory effect and fast charging. Therefore, they are widely used in electronic devices such as tablets, smart phones, laptops, game consoles, etc.

[0003] The reaction inside a lithium-ion secondary battery is mainly through the reciprocating movement of lithium ions between the positive electrode and the negative electrode to create a potential difference between the positive and negative electrodes. Generally, lithium-ion secondary batteries use graphite as the negative electrode material, and the energy density of lithium-ion secondary batteries using this negative electrode material is very low. Therefore, in order to improve the energy density, the industry has developed a variety of new negative electrode materials. Among them, the use of silicon oxide as the negative electrode material of lithium-ion secondary batteries can obtain high-voltage, high-energy-density lithium-ion secondary batteries.

[0004] The existing silicon oxide preparation device for preparing negative electrode materials of lithium secondary batteries generally comprises a raw material container, a heating device, a precipitation chamber and a vacuum device. The silicon oxide powder is placed in the raw material container and heated and gasified, and then the silicon oxide gas is extracted by the vacuum device and made to flow through the precipitation chamber to precipitate solid silicon oxide on the inner wall of the precipitation chamber. However, the yield of silicon oxide prepared by the existing silicon oxide preparation device is not good. Therefore, the existing silicon oxide preparation device is still not perfect in structural design and there is still room for improvement. Summary of the invention

[0005] In view of this, an object of the present invention is to provide a silicon oxide preparation device, which can increase the silicon oxide yield and facilitate users to take out the silicon oxide.

[0006] In order to achieve the above-mentioned purpose, the present invention provides a preparation device of silicon oxide, which includes a heating furnace, a heating device, a crucible, a deposition box, at least one exhaust pipe and a suction device. The interior of the heating furnace has a heating zone surrounded by a heat-insulating material; the heating device is arranged in the heating zone; the crucible is arranged in the heating zone to accommodate a solid raw material, and the solid raw material includes silicon dioxide and silicon. The heating device heats the crucible to form a gaseous silicon oxide from the solid raw material; the crucible has an upper opening; the deposition box is arranged between the heating zone and the inner furnace wall of the heating furnace, and the deposition The box has at least one air inlet and an air outlet, the deposition box includes at least one adsorbent and is arranged in the internal space of the deposition box, the surface material of the at least one adsorbent includes carbon; the at least one exhaust pipe has a first end and a second end, the first end is arranged at a position adjacent to the upper opening of the crucible, and the second end is connected to the at least one air inlet of the deposition box; and the exhaust device is connected to the air outlet of the deposition box; the exhaust device extracts the gaseous silicon oxide from the crucible so that the gaseous silicon oxide contacts the surface of the at least one adsorbent to deposit a solid silicon oxide.

[0007] The effect of the present invention is that, by providing the at least one adsorbent, the contact area between the deposition box and the gaseous silicon oxide can be increased, and the design that the surface material of the at least one adsorbent includes carbon can not only effectively increase the yield of silicon oxide precipitation, but also avoid the problem of metal contamination of the produced silicon oxide. BRIEF DESCRIPTION OF THE DRAWINGS

[0008] Figure 1 Schematic diagram of a silicon oxide preparation device according to a preferred embodiment of the present invention.

[0009] Figure 2 It is a schematic diagram of the partial decomposition of the components of the deposition box of the above preferred embodiment.

[0010] Figure 3 It is a schematic diagram of the box body of the deposition box of the above preferred embodiment.

[0011] Figure 4 It is a schematic diagram of partial decomposition of components of a deposition box according to another preferred embodiment.

[0012] Figure 5 A schematic diagram of a deposition box body according to another preferred embodiment.

[0013] Figure 6 FIG. 1 is a schematic diagram of a device for preparing silicon oxide according to another preferred embodiment.

[0014] Figure 7 A schematic diagram of a deposition box body according to another preferred embodiment.

[0015] Figure 8 FIG. 1 is a schematic diagram of the arrangement and distribution of adsorbents inside a deposition box according to another preferred embodiment. DETAILED DESCRIPTION

[0016] In order to more clearly illustrate the present invention, preferred embodiments are described in detail below with reference to the accompanying drawings. Figure 1 As shown, a silicon oxide preparation device 1 according to a preferred embodiment of the present invention comprises a heating furnace 10, a heating device 20, a crucible 30, a deposition box 40, an exhaust pipe 50 and a vacuum device 60.

[0017] The heating furnace 10 has a heating zone R formed by surrounding the heat insulating material 12. The heating device 20 and the crucible 30 are arranged in the heating zone R. The crucible 30 has an upper opening. The crucible 30 is used to accommodate a solid raw material. The solid raw material includes silicon dioxide and silicon. The heating device 20 includes a plurality of heaters, which are respectively arranged on the outer wall surrounding the crucible 30 and above the crucible 30. The heating device 20 is used to heat the crucible 30 so that the solid raw material forms a gaseous silicon oxide. In this embodiment, the heating device 20 can maintain the internal temperature of the heating zone R between 1300 and 1350 degrees.

[0018] The deposition box 40 is arranged between the heating zone R and the inner furnace wall of the heating furnace 10, and the deposition box 40 has an air inlet 40a and an air outlet 40b. The deposition box 40 includes a plurality of adsorbents 42 and is arranged in the internal space of the deposition box 40. The surface material of the plurality of adsorbents includes carbon. The thermal conductivity coefficient of the plurality of adsorbents 42 is greater than or equal to 16W / mK, and the melting point is greater than 1200 degrees. The exhaust pipe 50 has a first end 50a and a second end 50b. The first end 50a is arranged at a position adjacent to the upper opening of the crucible 30, and the second end 50b is connected to the air inlet 40a of the deposition box 40, and the exhaust device 60 is connected to the air outlet 40b of the deposition box 40. The exhaust device 60 can be, for example, a cyclone dust collector, through which gaseous silicon oxide can be precipitated in the cyclone dust collector, thereby improving the collection rate of solid silicon oxide. Thus, the exhaust device 60 can extract the gaseous silicon oxide from the crucible 30, so that the gaseous silicon oxide contacts the surface of the multiple adsorbents 42 to generate solid silicon oxide on the surface of the multiple adsorbents 42. The arrangement of the multiple adsorbents 42 and the design that the surface material of the multiple adsorbents 42 includes carbon can not only increase the contact area between the deposition box 40 and the gaseous silicon oxide to increase the yield of silicon oxide precipitation, but also avoid the problem of metal contamination of the produced silicon oxide. For example, the multiple adsorbents 42 can be components made of graphite or carbon / carbon composites. It should be noted that in other embodiments, the number of adsorbents 42 can also be one, and is not limited to the multiple adsorbents 42 in this embodiment. In this embodiment, the silicon oxide preparation device 1 includes a mask 70, the mask 70 covers the upper opening of the crucible 30, and the mask 70 has an opening 70a, the opening 70a communicates with the first end 50a of the exhaust pipe 50 and the interior of the crucible 30, and the mask 70 can limit the flow area of ​​the gaseous silicon oxide, thereby improving the collection rate of the solid silicon oxide. Figure 2 and Figure 3As shown, the deposition box 40 includes a box body 44, a partition 46 and a box cover 48, the box body 44 has a left side plate 441, a right side plate 442, a rear side plate 443, a top plate 444, a bottom plate 445 and a side opening 44a, the top plate 444 and the bottom plate 445 are arranged opposite to each other, the left side plate 441 and the right side plate 442 are arranged opposite to each other, the rear side plate 443 is respectively connected to the left side plate 441, the right side plate 442, the top plate 444 and the bottom plate 445, the top plate 444 has the air outlet 40b, the bottom plate 445 has the air inlet 40a, the partition 46 is arranged between the top plate 444 and the bottom plate 445, the multiple adsorbents 42 are arranged between the partition 46 and the bottom plate 445, and the box cover 48 is used to close the side opening 44a. One end edge of the partition 46 is connected to the rear side plate 443, and there is a distance D1 between the partition 46 and the side wall of the deposition box 40, that is, the left side plate 441 and the right side plate 442, respectively. The distance D1 is 5 to 10 cm, preferably 5 to 8 cm. Thereby, the gas outlet 40b and the gas inlet 40a can be connected through the distance D1. That is to say, after the gas enters the interior of the deposition box 40 from the gas inlet 40a of the deposition box 40, it passes through the distance D1 between the partition 46 and the left side plate 441 or the right side plate 442, and is discharged from the deposition box 40 from the gas outlet 40b. The spacing D1 is selected to be 5 to 10 cm in order to provide an appropriate gas flow rate to increase the collection rate of solid silicon oxide. When the spacing D1 is less than 5 cm, the gas entering the deposition box 40 from the gas inlet 40a is restricted by the spacing D1 and is difficult to flow, resulting in a too slow gas flow rate, which affects the yield of solid silicide generated on each of the adsorbents 42. When the spacing is greater than 10 cm, the gas entering the deposition box 40 from the gas inlet 40a can easily be quickly discharged from the deposition box 40 from the gas outlet 40b through the spacing D1, which will also affect the yield of solid silicide generated on each of the adsorbents 42.

[0019] In this embodiment, the partition 46 is connected to the rear side plate 443 and there is a distance D1 between the partition 46 and the left side plate 441 and the right side plate 442. In other embodiments, it is not excluded that the partition 46 can also be connected to at least one of the left side plate 441, the right side plate 442 or the rear side plate 443, and there is a distance D1 between the partition 46 and at least one of the left side plate 441, the right side plate 442 or the rear side plate 443 of the deposition box 40, which can also achieve the effect of connecting the gas outlet 40b and the gas inlet 40a. In addition, if Figure 4As shown, the partition 46 may also be connected to the box cover 48, whereby when the user opens the box cover 48, each of the adsorbents 42 can be taken out from the box body 44 of the deposition box 40 at the same time, so that the solid silicide products generated on each of the adsorbents 42 can be smoothly obtained. In this embodiment, the user manually scrapes off each of the adsorbents 42 with a scraper to obtain the solid silicide products generated on each of the adsorbents 42. In other embodiments, it is not excluded that a scraper is provided in the deposition box 40 to automatically scrape off each of the adsorbents 42 to obtain the solid silicide products generated on each of the adsorbents 42.

[0020] Each of the adsorbents 42 is in the shape of a rod, and the diameter X of the plurality of adsorbents 42 is between 0.5 and 1 cm, the length H is between 15 and 20 cm, the spacing Y between the adsorbents 42 is between 3 and 5 cm, and the two ends of the rod body of each adsorbent 42 respectively have a third end 42a and a fourth end 42b opposite to each other, and the fourth end 42b is arranged at a position close to the gas inlet 40a relative to the third end 42a, thereby increasing the contact area between the deposition box 40 and the gaseous silicon oxide. In this embodiment, the third end 42a of the plurality of adsorbents 42 is connected to the partition 46, and in other embodiments, it can also be as follows Figure 5 As shown, the partition 46 is not provided, and each of the adsorbents 42 can be directly connected to the top plate 444 of the deposition box 40. It should be noted that in this embodiment, each of the adsorbents 42 is detachably provided in the deposition box 40. For example, each of the adsorbents 42 can be screwed together with the partition 46, so that the user can take each of the adsorbents 42 out of the deposition box 40 to facilitate obtaining the solid silicide product generated on each of the adsorbents 42. In the present embodiment, each of the adsorbents 42 is disposed in the deposition box 40 so as to be non-movable relative to the deposition box 40. In other embodiments, it is not excluded that each of the adsorbents 42 is disposed in the deposition box 40 so as to be movable relative to the deposition box 40. For example, the adsorbent 42 disposed at a position close to the air inlet 40a can be moved to a position away from the air inlet 40a, and another adsorbent 42 disposed at a position away from the air inlet 40a can be moved to a position close to the air inlet 40a, thereby improving the collection rate of solid silicon oxide.

[0021] Please cooperate again Figure 3, one of the plurality of adsorbents 42 has a long axis and the extension line L of the long axis passes through the air inlet 40a, that is, the adsorbent 42 is arranged above the air inlet 40a, and the adsorbent 42 and the air inlet 40a are separated by a distance D2, that is, the minimum distance between the adsorbent 42 and the bottom plate 445, and the distance D2 is 3 to 13 cm. The distance D2 is selected to be 3 to 13 cm because the minimum distance between each adsorbent 42 and the bottom plate 445 is 3 to 13 cm, which can obtain the preferred solid silicide yield of a single adsorbent. According to the experimental data of the inventor According to the experimental data, when the minimum distance between each adsorbent 42 and the bottom plate 445 is 6 cm and 10 cm, the solid silicide yield rate of a single adsorbent is 37% and 35% respectively; when the minimum distance between each adsorbent 42 and the bottom plate 445 is 3 cm, the solid silicide yield rate of a single adsorbent is 11%; when the minimum distance between each adsorbent 42 and the bottom plate 445 is 13 cm and 15 cm, the solid silicide yield rate of a single adsorbent is 13% and 6% respectively. It can be seen from the above experimental data that the distance D2 is preferably 6 to 10 cm, which can obtain the best solid silicide yield rate of a single adsorbent.

[0022] In addition, in this embodiment, the length H of the multiple adsorbents 42 is set according to the distance between each of the adsorbents 42 and the air inlet 40a. The length H of the adsorbent 42 that is closer to the air inlet 40a must be shorter than the length of the adsorbent 42 that is farther away from the air inlet 40a. In this way, not only can the contact probability between the adsorbent 42 and the gaseous silicon oxide be increased, but also the solid silicide generated on the adsorbent 42 can be prevented from clogging the air inlet 40a.

[0023] In this embodiment, the deposition box 40 is provided with an air inlet 40a and an exhaust pipe 50. In practice, the deposition box 40 may also be provided with a plurality of air inlets 40a and a plurality of exhaust pipes 50. Figure 6 and Figure 7 The deposition box 40 may also be provided with three air inlets 40a, and three exhaust pipes 50 are provided correspondingly, wherein the long axial extension lines L of the three adsorbents 42 respectively pass through the multiple air inlets 40a and are separated from the corresponding air inlets 40a by a distance, thereby increasing the contact probability and contact area between the adsorbent 42 and the gaseous silicon oxide, thereby greatly improving the yield of solid silicon oxide. In other embodiments, the number of air inlets and exhaust pipes may be two or more than three.

[0024] It is further explained that in this embodiment, the plurality of adsorbents 42 are arranged in a row at a distance from each other. In practice, the plurality of adsorbents can also be arranged in an array or various arrangement patterns, or the plurality of adsorbents can be arranged at unequal intervals from each other. For example, compared with the adsorbents arranged above the air inlet 40a, the adsorbents arranged above the air inlet 40a can be arranged at a closer distance from each other, and the above embodiment is not limited thereto. Figure 8 The present invention is a schematic diagram of the arrangement and distribution of adsorbents in a deposition box according to another embodiment, wherein adsorbents 421, 422, 423, 424, 425, 426 and 427 are the rod-shaped adsorbents described in the above embodiments, and adsorbent 428 is a thin plate-shaped adsorbent. Please refer to Table 1 below for the solid silicide yield rate (%) of each adsorbent in the deposition box. According to Table 1, it can be seen that adsorbent 428 is a thin plate-shaped adsorbent, which can also make gaseous silicon oxide contact with the surface of adsorbent 428 to generate solid silicon oxide on the thin plate surface of adsorbent 428. It is worth mentioning that the long axial extension line L of adsorbent 423 passes through the air inlet 40a, that is, the adsorbent 423 is arranged above the air inlet 40a. As shown in Table 1, the adsorbent 423 can obtain the preferred solid silicide yield rate of a single adsorbent by being arranged above the air inlet 40a.

[0025] Table 1

[0026] Adsorption parts Solid silicide yield% Adsorption parts 421, 424, 425, 427 3.00％ Adsorption parts 422 4.10％ Adsorption parts 423 16.80％ Adsorption parts 428 1.80％ Adsorption parts 426 5.30％

[0027] In summary, by configuring the multiple adsorbents 42 of the present invention, the contact area between the deposition box 40 and the gaseous silicon oxide can be increased, and the design that the surface material of the multiple adsorbents includes carbon can not only effectively increase the yield of silicon oxide precipitation, but also avoid the problem of metal contamination of the produced silicon oxide. The above is only a preferred feasible embodiment of the present invention, and any equivalent changes made by applying the present invention specification and the scope of the patent application should be included in the patent scope of the present invention.

[0028] Description of Reference Numerals

[0029] [The present invention]

[0030] 1: Silicon oxide preparation device

[0031] 10: Heating furnace

[0032] 12: Thermal insulation material

[0033] 20: Heating device

[0034] 30: Crucible

[0035] 40a: Air inlet

[0036] 40b: Air outlet

[0037] 40: Sedimentation Box

[0038] 42: Adsorption parts

[0039] 42a: The third end

[0040] 42b: The fourth end

[0041] 44: Box

[0042] 441: Left side panel

[0043] 442: Right side panel

[0044] 443: Rear side panel

[0045] 444: Top plate

[0046] 445: Base plate

[0047] 44a: Side opening

[0048] 46: Partition

[0049] 48: Lid

[0050] 50: Exhaust duct

[0051] 50a: First end

[0052] 50b: Second end

[0053] 60: Vacuum device

[0054] 70: Mask

[0055] 70a: Open hole

[0056] D1: Spacing

[0057] D2: Distance

[0058] H: Length

[0059] L: Extension line

[0060] R: Heating zone

[0061] X: Diameter

[0062] Y: Spacing

Claims

1. A device for preparing silicon oxide, comprising: A heating furnace having a heating zone surrounded by a heat insulating material; a heating device, disposed in the heating zone; a crucible, disposed in the heating zone, for containing a solid raw material, the solid raw material comprising silicon dioxide and silicon, the crucible having an upper opening; A deposition box is disposed between the heating zone and the inner furnace wall of the heating furnace, the deposition box has at least one air inlet and an air outlet, the deposition box includes at least one adsorbent and is disposed in the inner space of the deposition box, and the surface material of the at least one adsorbent includes carbon; at least one exhaust duct having a first end and a second end, wherein the first end is disposed adjacent to the upper opening of the crucible, and the second end is connected to the at least one gas inlet of the deposition box; and an exhaust device, connected to the gas outlet of the deposition box; Wherein, the at least one adsorbent is spaced from the at least one air inlet by a distance, and the distance is 3 to 13 cm; Wherein, the at least one adsorption member has a long axial direction, and an extension line of the long axial direction passes through the at least one air inlet; Among them, the number of the at least one adsorbent is multiple, one of the multiple adsorbents has the long axis, and the length of the adsorbent among the multiple adsorbents that is closer to the air inlet must be shorter than the length of the adsorbent among the multiple adsorbents that is farther away from the air inlet.

2. The silicon oxide preparation device according to claim 1, wherein: The at least one adsorbent is in a rod shape and has a third end and a fourth end opposite to each other. The fourth end is arranged at a position close to the at least one air inlet relative to the third end.

3. The device for preparing silicon oxide according to claim 2, wherein: The deposition box includes a partition and a top plate and a bottom plate arranged opposite to each other, the top plate has the gas outlet, the bottom plate has the at least one gas inlet, the partition is arranged between the top plate and the bottom plate, the at least one adsorbent is arranged between the partition and the bottom plate, and the third end of the at least one adsorbent is connected to the partition.

4. The device for preparing silicon oxide according to claim 3, wherein: There is at least one gap between the partition and the side wall of the deposition box, and the gas outlet is connected to the at least one gas inlet through the at least one gap.

5. The device for preparing silicon oxide according to claim 4, wherein: The deposition box comprises a box body and a box cover, wherein the box body has a side opening, the box cover is used to close the side opening, and the partition is connected to the box cover.

6. The device for preparing silicon oxide according to claim 1, wherein: The plurality of adsorption elements are arranged in a manner of being spaced apart from each other by a distance.

7. The device for preparing silicon oxide according to claim 1, wherein: The deposition box includes a top plate and a bottom plate that are arranged opposite to each other, the top plate has the gas outlet, the bottom plate has the at least one gas inlet, and the at least one adsorbent is connected to the top plate.

8. The device for producing silicon oxide according to any one of claims 1 to 7, wherein: The at least one adsorbent is made of graphite or a carbon / carbon composite material.

9. The silicon oxide preparation device as claimed in claim 4, wherein: The at least one distance is 5 to 10 centimeters.

10. The silicon oxide preparation device according to claim 1, wherein: The at least one air inlet and the at least one exhaust pipe are respectively plural in number and are correspondingly connected.

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