TW202246178A - Silicon oxide preparation device - Google Patents

Abstract

A silicon oxide preparation device includes a heating furnace, a heating device, a crucible, a deposition box, at least one exhaust pipe, and an exhaust device. The crucible and the deposition box are set in the heating furnace, and the heating The device heats the crucible so that the solid raw material contained in the crucible forms a gaseous silicon oxide. The deposition box has at least one gas inlet and one gas 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 opening on the crucible, the second end of the at least one exhaust pipe is communicated with at least one air inlet of the deposition box; The air exhaust device communicates with the air outlet of the deposition box to extract the gaseous silicon oxide from the crucible and contact the gaseous silicon oxide with the surface of the at least one adsorbent to deposit a solid silicon oxide.

Description

Preparation device of silicon oxide

The present invention is related to the preparation device of silicon oxide; in particular, it refers to a preparation device capable of increasing the output of silicon oxide.

Known secondary batteries include nickel-cadmium batteries, nickel-hydrogen batteries, lithium-ion secondary batteries, etc., and lithium-ion secondary batteries have high energy density, high operating voltage, and small memory effect compared with nickel-cadmium batteries or nickel-hydrogen batteries. As well as features such as fast charging, it is widely used in electronic devices such as tablet computers, smart phones, notebook computers, and game consoles.

The reaction inside the 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 electrode and the negative electrode. The general lithium ion secondary battery mostly uses graphite as the negative electrode material, and this negative electrode is used The energy density of lithium-ion secondary batteries is very low. Therefore, in order to increase energy density, the industry has developed a variety of new negative electrode materials. Among them, silicon oxide can be used as the negative electrode material of lithium-ion secondary batteries to obtain high voltage and high energy density. Lithium-ion secondary battery.

The conventional silicon oxide preparation device used to prepare negative electrode materials for lithium secondary batteries usually includes a raw material container, a heating device, a precipitation chamber and an air extraction device, by placing the powder containing silicon oxide in the raw material container And after heating and vaporizing, the silicon oxide gas is extracted by the pumping device and made to flow through the precipitation chamber to precipitate solid silicon oxide on the inner wall of the precipitation chamber, but it is prepared by using a conventional silicon oxide preparation device The yield of silicon oxide is not good. Therefore, the structural design of conventional silicon oxide preparation devices is still not perfect, and there is still room for improvement.

In view of this, the purpose of the present invention is to provide a silicon oxide preparation device, which can increase the output of silicon oxide and facilitate users to take out silicon oxide.

In order to achieve the above object, a silicon oxide preparation device provided by the present invention includes a heating furnace, a heating device, a crucible, a deposition box, at least one exhaust pipe and an exhaust device, and the heating furnace is equipped with a A heat-insulating material surrounds and forms a heating area; the heating device is arranged in the heating area; the crucible is arranged in the heating area for accommodating a solid raw material, the solid raw material includes silicon dioxide and silicon, the The heating device heats the crucible to make the solid raw material form a gaseous silicon oxide; the crucible has an upper opening; the deposition box is arranged between the heating zone and the inner wall of the heating furnace, and the deposition box has at least one inlet Gas port and a gas outlet, the deposition box includes at least one adsorption piece and is arranged in the inner space of the deposition box, the surface material of the at least one adsorption piece includes carbon; the at least one exhaust pipe has a first end and a a second end, the first end is disposed adjacent to the upper opening of the crucible, the second end communicates with the at least one gas inlet of the deposition box; and the air extraction device communicates with the gas outlet of the deposition box; The gas pumping device sucks the gaseous silicon oxide out of the crucible, so that the gaseous silicon oxide contacts the surface of the at least one adsorbent to deposit a solid silicon oxide.

The effect of the present invention is that the contact area between the deposition box and gaseous silicon oxide can be increased by the arrangement of the at least one adsorbent, and the design of the surface material of the at least one adsorbent including carbon can not only effectively improve the precipitation of silicon oxide The output can also avoid the problem of metal contamination of the silicon oxide produced.

In order to illustrate the present invention more clearly, preferred embodiments are given and detailed descriptions are given below in conjunction with drawings. Please refer to Fig. 1, which is a silicon oxide preparation device 1 of a preferred embodiment of the present invention, comprising a heating furnace 10, a heating device 20, a crucible 30, a deposition box 40, an exhaust pipe 50 and A suction device 60.

The inside of the heating furnace 10 has a heating zone R surrounded by a 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, and the crucible 30 is used for 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 around the outer side wall of the crucible 30 and above the crucible 30, the heating device 20 is The crucible 30 is used to heat the solid raw material to form 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.

The deposition box 40 is arranged between the heating zone R and the inner furnace wall of the heating furnace 10. The deposition box 40 has a gas inlet 40a and a gas outlet 40b. The deposition box 40 includes a plurality of adsorption parts 42 and is arranged on In the inner space of the deposition box 40, the surface material of the adsorbents includes carbon, the thermal conductivity of the adsorbents 42 is greater than or equal to 16W/m.K, 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 disposed adjacent to the upper opening of the crucible 30, the second end 50b communicates with the gas inlet 40a of the deposition box 40, and the air extraction device 60 is connected to the The gas outlet 40b of the deposition box 40 is connected, and the air extraction device 60 can be, for example, a cyclone dust collector, through which the gaseous silicon oxide can be separated out in the cyclone dust collector, thereby improving the solid silicon oxide. collection rate. Thereby, the gas extraction device 60 can extract the gaseous silicon oxide from the crucible 30, so that the gaseous silicon oxide contacts the surfaces of the adsorbents 42 to generate solid silicon on the surfaces of the adsorbents 42. oxide, and through the arrangement of these adsorbents 42 and the design of the surface material of these adsorbents 42 including carbon, not only can the contact area between the deposition box 40 and gaseous silicon oxide be increased to improve the yield of silicon oxide precipitation, It can also avoid the problem of metal contamination of the produced silicon oxide. For example, the adsorbents 42 can be components made of graphite or carbon/carbon composite. It should be noted that, in other embodiments, the number of the adsorption member 42 may also be one, and is not limited to the plurality of adsorption members 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, and the opening 70a communicates with the The first end 50a of the exhaust pipe 50 and the inside of the crucible 30 can limit the flow area of the gaseous silicon oxide through the arrangement of the shield 70, thereby improving the collection rate of the solid silicon oxide.

In this embodiment, as shown in Figure 2 and Figure 3, 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 one side opening 44a, the top plate 444 and the bottom plate 445 are arranged oppositely, the left side plate 441 and the right side plate 442 are arranged oppositely, 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 plate 46 is arranged between the top plate 444 and the bottom plate 445, these The absorber 42 is disposed between the partition 46 and the bottom plate 445 , and the box cover 48 is used to close the side opening 44 a. Wherein one end edge of the partition plate 46 is connected to the rear side plate 443, and there is a distance D1 between the partition plate 46 and the side wall of the deposition box 40, that is, between the left side plate 441 and the right side plate 442, and the distance D1 is 5 ~10cm, preferably 5~8cm, whereby the gas outlet 40b and the gas inlet 40a can communicate through the distance D1, that is to say, the gas can enter the deposition box 40 from the gas inlet 40a of the deposition box 40 After the inside, the deposition box 40 is discharged from the gas outlet 40 b through the distance D1 between the partition 46 and the left side plate 441 or the right side plate 442 respectively. The purpose of choosing the distance D1 to be 5-10 cm is to provide an appropriate gas flow rate to improve the collection rate of solid silicon oxide. When the distance D1 is less than 5 cm, the gas entering the deposition box 40 from the gas inlet 40a is limited by the distance D1 Restricted and difficult to circulate, the gas flow rate is too slow, which affects the solid-state silicide yield generated on each of the adsorbents 42, and when the distance is greater than 10cm, the gas entering the deposition box 40 from the gas inlet 40a is easy to pass through the The rapid discharge of the deposition box 40 from the gas outlet 40 b at the distance D1 will also affect the yield of solid silicide formed on each of the adsorbents 42 .

In this embodiment, it is illustrated by taking that the partition plate 46 is connected to the rear side plate 443 and that there is a distance D1 between the partition plate 46 and the left side plate 441 and the right side plate 442 respectively. In other embodiments, no Excluding the partition plate 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 the partition plate 46 and the left side plate 441, the right side plate 442 of the deposition box 40 Or there is a distance D1 between at least one of the rear side panels 443, which can also achieve the effect of communicating the air outlet 40b and the air inlet 40a. In addition, as shown in FIG. 4 , the partition 46 can also be connected to the box cover 48, whereby when the user opens the box cover 48, each of the adsorbents 42 can be deposited from the box at the same time. Take it out from the box body 44 of the box 40, 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 product formed on each of the adsorbents 42. In other embodiments, the deposition box 40 is not excluded. The scraper automatically scrapes off each of the adsorbents 42 to obtain the solid silicide products generated on each of the adsorbents 42 .

Wherein, each of the adsorbents 42 is rod-shaped, the diameter X of the adsorbents 42 is between 0.5 and 1 cm, the length H is between 15 and 20 cm, and the distance Y between the adsorbents 42 is between 3 and 5 cm. , and the two ends of the rod body of each of the adsorbents 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 air inlet 40a relative to the third end 42a, In this way, the contact area between the deposition box 40 and the gaseous silicon oxide is increased. In this embodiment, the third ends 42a of the adsorbents 42 are connected to the partition 46. In other embodiments, as shown in FIG. 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 arranged in the deposition box 40. For example, each of the adsorbents 42 can be combined with the compartment by screwing. In this way, the user can take out each of the adsorption pieces 42 from the deposition box 40, so as to obtain the solid silicide products generated on each of the adsorption pieces 42. In this embodiment, each of the adsorption pieces 42 is installed in the deposition box 40 so that it cannot move relative to the deposition box 40. In other embodiments, it is not excluded that each of the adsorption pieces 42 can move relative to the deposition box 40 The method is arranged in the deposition box 40, for example, the adsorption member 42 arranged at the position close to the gas inlet 40a can be moved to a position away from the gas inlet 40a, and is arranged at a position far away from the gas inlet 40a. Another adsorption member 42 can be moved to a position close to the air inlet 40a, thereby improving the collection rate of solid silicon oxide.

Please cooperate with FIG. 3 again, one of the adsorbents 42 has a long axis and the extension line L of the long axis passes through the air inlet 40a, that is to say, the adsorbent 42 is arranged on the air inlet 40a. above, and there is a distance D2 between the adsorbent 42 and the air inlet 40a, that is, the minimum distance between the adsorbent 42 and the bottom plate 445, the distance D2 is 3~13 centimeters, and the distance D2 is 3~13 centimeters It is because the minimum distance between each of the adsorbents 42 and the bottom plate 445 is 3 to 13 centimeters to obtain a better solid-state silicide output rate of a single adsorber. According to the experimental data of the inventor, when each of the adsorbents 42 and the bottom plate When the minimum distance between 445 is 6 cm and 10 cm, the solid silicide output rate of a single adsorbent is 37% and 35%, respectively. When the minimum distance between each of the adsorbents 42 and the bottom plate 445 is 3 cm, the The output rate of solid silicide is 11%. When the minimum distance between each of the adsorption parts 42 and the bottom plate 445 is 13 cm and 15 cm, the output rate of solid silicide for a single adsorption part is 13% and 6%, respectively. Through From the above experimental data, it can be known that the distance D2 is preferably 6-10 cm, which can obtain the best yield rate of solid silicide for a single adsorbent.

In addition, in this embodiment, the length H of the adsorbents 42 is set according to the distance between each adsorbent 42 and the air inlet 40a, and the closer the distance to the air inlet 40a is the length of the adsorbent 42 H 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 avoid the formation of the adsorbent 42 on the adsorbent 42. Solid silicide blocks the gas inlet 40a.

In this embodiment, the deposition box 40 has an air inlet 40a and an exhaust pipe 50 is provided as an example. In practice, the deposition box 40 can also be provided with a plurality of air inlets 40a, and a plurality of corresponding One exhaust duct 50, for example, please cooperate with Fig. 6 and Fig. 7, this deposition box 40 also can be provided with three gas inlets 40a, and correspondingly arrange three exhaust ducts 50, wherein the major axis of three adsorbents 42 The extended lines L in the direction respectively pass through the gas inlets 40a and are separated from the corresponding gas 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 solid silicon oxide. output. In other embodiments, the number of air inlets and exhaust pipes can be two or more than three respectively.

It should be further explained that, in this embodiment, the adsorbents 42 are arranged in a row at a distance from each other as an example. In practice, the adsorbents can also be arranged in an array or Various arrangement patterns, or the adsorbents are 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 The components can be arranged in a manner with a relatively close distance from each other, which is not limited to the above-mentioned embodiments. Please refer to FIG. 8 for a schematic diagram of the arrangement and distribution of the adsorption parts in the deposition box according to another embodiment, wherein the adsorption parts 421, 422, 423, 424, 425, 426 and 427 are For the rod-shaped adsorbent described in the above embodiment, the adsorbent 428 is a thin plate-shaped adsorbent. Please cooperate with the following table 1, which is the solid silicide yield % of each adsorbent in the deposition box. According to Table 1, it can be seen that the adsorbent 428 The thin plate-shaped adsorbent can also make the gaseous silicon oxide contact with the surface of the adsorbent 428 to generate solid silicon oxide on the surface of the adsorbent 428 thin plate. It is worth mentioning that the long axis extension line of the adsorbent 423 L passes through the air inlet 40a, that is to say, the adsorbent 423 is arranged above the air inlet 40a, as shown in Table 1, the adsorbent 423 can obtain a better single adsorbent by being arranged above the air inlet 40a The solid silicide yield %.

Table 1 Adsorbent Solid silicide yield % Adsorbents 421, 424, 425, 427 3.00% Adsorbent 422 4.10% Adsorbent 423 16.80% Adsorbent 428 1.80% Adsorbent 426 5.30%

To sum up, through the arrangement of these adsorbents 42 of the present invention, the contact area between the deposition box 40 and gaseous silicon oxide can be increased, and the design of the surface material of these adsorbents includes carbon can not only effectively improve silicon oxide The yield of precipitation can also avoid the problem of metal contamination of the produced silicon oxide. The above description is only a preferred feasible embodiment of the present invention, and all equivalent changes made by applying the description of the present invention and the scope of the patent application should be included in the scope of the patent of the present invention.

[this invention] 1: Preparation device of silicon oxide 10: Heating furnace 12: Insulation material 20: Heating device 30: Crucible 40a: air inlet 40b: Air outlet 40: deposition box 42: Adsorption parts 42a: third end 42b: the fourth end 44: box body 441: left panel 442: Right side panel 443: Rear side panel 444: top plate 445: bottom plate 44a: side opening 46: Partition 48: box cover 50: exhaust pipe 50a: first end 50b: second end 60: Air extraction device 70: mask 70a: opening D1: Spacing D2: distance H: Length L: extension line R: heating zone X: diameter Y: Spacing

FIG. 1 is a schematic diagram of a silicon oxide preparation device according to a preferred embodiment of the present invention. Fig. 2 is an exploded schematic diagram of some components of the deposition box of the above-mentioned preferred embodiment. Fig. 3 is a schematic diagram of the box body of the deposition box of the above-mentioned preferred embodiment. FIG. 4 is an exploded schematic diagram of some components of a deposition box in another preferred embodiment. Fig. 5 is a schematic diagram of a box body of a deposition box in another preferred embodiment. FIG. 6 is a schematic diagram of a silicon oxide preparation device in another preferred embodiment. Fig. 7 is a schematic diagram of a box body of a deposition box in another preferred embodiment. Fig. 8 is a schematic diagram showing the arrangement and distribution of the adsorption components inside the deposition box according to another preferred embodiment.

1: Preparation device of silicon oxide

10: Heating furnace

12: Insulation material

20: Heating device

30: Crucible

40a: air inlet

40b: Air outlet

40: deposition box

42: Adsorption parts

50: exhaust pipe

50a: first end

50b: second end

60: Air extraction device

70: mask

70a: opening

R: heating zone

Claims (14)

A silicon oxide preparation device, comprising: A heating furnace with a heating zone formed inside by a heat insulating material; a heating device arranged in the heating zone; A crucible, arranged in the heating zone, is used to accommodate a solid raw material, the solid raw material includes silicon dioxide and silicon, and the crucible has an upper opening; A deposition box is arranged between the heating zone and the inner furnace wall of the heating furnace, the deposition box has at least one gas inlet and one gas outlet, the deposition box includes at least one adsorption piece and is arranged in the inner space of the deposition box wherein, the surface material of the at least one adsorbent comprises carbon; At least one exhaust pipe has a first end and a second end, the first end is disposed adjacent to the upper opening of the crucible, and the second end communicates with the at least one gas inlet of the deposition box; and A gas extraction device communicated with the gas outlet of the deposition box. The device for preparing silicon oxide according to claim 1, wherein the at least one adsorption member is separated from the at least one gas inlet by a distance. The device for preparing silicon oxide according to claim 2, wherein the distance between the at least one adsorption member and the at least one gas inlet is 3-13 cm. The device for preparing silicon oxide according to claim 2, wherein the at least one adsorbent has a long axis, and the extension of the long axis passes through the at least one gas inlet. The device for preparing silicon oxide according to claim 4, wherein the at least one adsorption member is plural in number, and one of the adsorption members has the long axis. The device for preparing silicon oxide according to claim 4, wherein the at least one adsorption member is rod-shaped, the at least one adsorption member has a third end and a fourth end opposite to each other, and the fourth end is opposite to the third end. The end is disposed close to the at least one air inlet. The device for preparing silicon oxide according to claim 6, wherein the deposition box includes a partition and a top plate and a bottom plate oppositely arranged, the top plate has the gas outlet, the bottom plate has the at least one gas inlet, and the partition The board is arranged between the top board and the bottom board, the at least one adsorption piece is arranged between the partition board and the bottom board, and the third end of the at least one suction piece is connected to the partition board. The device for preparing silicon oxide according to claim 7, wherein there is at least a gap between the partition and the side wall of the deposition box, and the gas outlet communicates with the at least one gas inlet through the at least one gap. The device for preparing silicon oxide according to claim 8, wherein the deposition box includes a box body and a box cover, the box body has a side opening, the box cover is used to close the side opening, and the partition is connected to The lid on the box. The device for preparing silicon oxide according to claim 4, wherein the adsorbents are arranged at a distance from each other. The device for preparing silicon oxide according to claim 1, wherein the deposition box includes a top plate and a bottom plate oppositely arranged, the top plate has the gas outlet, the bottom plate has the at least one gas inlet, and the at least one adsorption member is connected to on the top plate. The device for preparing silicon oxide according to any one of claims 1 to 11, wherein the at least one adsorbent is made of graphite or carbon/carbon composite. The silicon oxide manufacturing device as described in claim 8, wherein the at least one distance is 5-10 cm. The device for preparing silicon oxide according to claim 1, wherein the at least one air inlet and the at least one exhaust pipe are plural in number and communicated correspondingly.

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