Purification method and purification processing system of diiodosilane

Abstract

The invention discloses a diiodosilane purification method and a purification processing system, and relates to the technical field of diiodosilanes. A driving assembly is arranged on a mounting shell, an inner container piece is clamped to the output end of the driving assembly, the driving assembly is in sliding connection with a sliding groove formed in the mounting shell, the inner container piece is located in a sliding cavity in the mounting shell, and the inner container piece is connected with the driving assembly in a sliding mode; the sliding cavity is communicated with the sliding groove, a limiting assembly is mounted on the mounting shell, a notch is formed in the mounting shell, the limiting assembly inclines towards the notch, crystals can be rapidly taken out by taking out the inner container piece, the working efficiency is improved, the crystals can be rapidly taken out conveniently, the next time of crystallization can be rapidly carried out, and the crystallization efficiency is improved. And a filter screen and a handrail are arranged on the inner container piece, so that residual liquid in the inner container piece can quickly flow out, and the residual liquid is prevented from influencing the purity of diiodosilane.

Description

Technical Field

[0001] The present invention relates to the technical field of diiodosilane, and specifically to a purification method and a purification processing system for diiodosilane. Background Art

[0002] Diiodosilane (DIS) is an advanced silicon-based precursor material, mainly used in semiconductor manufacturing and thin film deposition. The molecular formula of diiodosilane is H2I2Si, and it has multiple synthesis routes, including synthesis methods using silane and hydrogen iodide, diphenylsilane and hydrogen iodide, phenylsilane and elemental iodine, etc. as raw materials;

[0003] After retrieval, the patent with the publication number CN221789299U is a reaction kettle for producing diiodosilane, which includes a kettle body. An interconnected heating chamber and a reaction chamber are provided inside the kettle body, and a raised end is provided at the bottom of the reaction chamber; a cover plate, which is connected to the upper end of the kettle body; a mixing mechanism, including a driving part, a stirring part, and a plurality of material conveying cylinders; the driving part is arranged above the cover plate and is used to drive the stirring part arranged in the reaction chamber to mix and stir the materials; the material conveying cylinders are arranged in the heating chamber and are used to return the materials to the reaction chamber, and a plurality of heating parts are arranged in the heating chamber. It solves the technical problem that in the existing reaction kettle, when mixing the raw materials for making diiodosilane, the stirring efficiency is low, resulting in some materials being easily deposited at the bottom of the reaction kettle, thus affecting the quality of the subsequent products;

[0004] However, the crude diiodosilane needs to be purified. Therefore, it needs to be crystallized and purified. However, the crystallized diiodosilane will adhere to the reaction chamber, making it difficult to take out the crystals. Moreover, at this time, the diiodosilane is at a low temperature and cannot be easily touched, further increasing the difficulty of taking out the crystals. Summary of the Invention

[0005] The purpose of the present invention is to provide a purification method and a purification processing system for diiodosilane to solve the deficiencies in the above-mentioned prior art.

[0006] To achieve the above purpose, the present invention provides the following technical solutions:

[0007] The following steps are carried out:

[0008] S1. Collect the crude diiodosilane liquid;

[0009] S2. Distill the crude diiodosilane liquid. The boiling point of diiodosilane is about 210°C;

[0010] S3. Collect the fraction after condensation to remove low-boiling impurities;

[0011] S4. Freeze and crystallize the fraction after distillation. The freezing point of diiodosilane is about -57°C;

[0012] S5. Filter to obtain crystals to remove high-boiling impurities;

[0013] S6. Add a reagent that can react with impurities and does not affect disilane diiodide;

[0014] S7. Perform distillation and filtration separation to remove residual impurities.

[0015] Furthermore, it includes an installation shell, on which a driving component is provided. A liner part is clamped at the output end of the driving component. The driving component is slidably connected to a sliding groove opened on the installation shell. The liner part is located in a sliding cavity inside the installation shell. The sliding cavity is communicated with the sliding groove. The sliding cavity can collect the fractions in S and can withstand freezing to crystallize the fractions;

[0016] A limiting component is installed on the installation shell. A notch is opened on the installation shell. The inclined direction of the limiting component faces the notch.

[0017] Furthermore, the driving component includes an electric telescopic rod provided on the installation shell. The output end of the electric telescopic rod is rotatably connected to a disc part. The disc part is penetrated and fixedly connected by four clamping columns. Two first spring telescopic parts are provided on each of the four clamping columns. An inclined block is provided at the output end of each of the several first spring telescopic parts.

[0018] Furthermore, two second spring telescopic parts are fixed on each of the four clamping columns. A connecting part is provided at the output end of each of the several second spring telescopic parts. The several connecting parts are respectively fixedly connected to one end of several first wires. The other ends of the several first wires are respectively connected to the several inclined blocks.

[0019] Furthermore, the driving component further includes a limiting block fixedly provided on the disc part. The limiting block is slidably connected in the sliding groove.

[0020] Furthermore, the bottom of the liner part is set as a filter screen. The side of the liner part is provided with several railings. Four clamping parts are provided on the liner part. Four clamping grooves are respectively opened on the four clamping parts. The four clamping grooves respectively correspond to the positions of the four clamping columns.

[0021] Furthermore, the limiting component includes two limiting units. Each limiting unit includes two third spring telescopic parts fixedly provided inside the installation shell. A limiting part is provided at the output ends of the two third spring telescopic parts. The limiting part penetrates into the sliding cavity. An inclined surface is provided on the limiting part. The inclined direction of the inclined surface faces the notch. The limiting part is fixedly connected to one end of a second wire.

[0022] Further, one end of each of the two second wires away from the limiting member is fixedly connected to a pressing block, the pressing block is fixedly arranged at the output end of a fourth spring telescopic member, and the fourth spring telescopic member is fixedly arranged on the mounting shell.

[0023] Further, a slope is arranged on the mounting shell, the slope is connected to the two inclined surfaces, the slope is located at the sliding groove, and a storage box is arranged on the mounting shell, and the storage box corresponds to the position of the sliding groove.

[0024] Further, an inclined surface is arranged on the bottom surface of each of the two limiting members.

[0025] In the above technical solution, a purification method and a purification processing system for diiodosilane provided by the present invention place the inner liner member under the disc member, so that the four clamping grooves respectively correspond to the four clamping posts. Then, the inner liner member is lifted upward, so that the four clamping members are respectively clamped with the four clamping posts one by one. The diiodosilane solution to be purified is injected into the sliding cavity. Then, the electric telescopic rod is started to drive the disc member to move downward, and at the same time, sealing rubber rings are arranged on the four sides of the disc member, so that the diiodosilane solution to be purified is sealed. Then, the diiodosilane solution to be purified is crystallized. The crystallized diiodosilane will adhere to the inside of the sliding cavity. Before moving downward, press the pressing block, so that the fourth spring telescopic member contracts, driving the two second wires to be pulled, so that the two limiting members are pulled, so that the presence of the limiting members does not affect the downward movement of the inner liner member. Then, the electric telescopic rod is started to drive the disc member to move upward. Through the arrangement of the sliding groove, the limiting block rotates when moving upward, driving the inner liner member to rotate, so that the diiodosilane crystal no longer adheres to the inner liner of the sliding cavity, so that the inner liner member can be quickly taken out, so that the crystal can be quickly taken out, enhancing the working efficiency, facilitating the quick taking out of the crystal, enabling the next crystallization to be carried out quickly, and through the arrangement of the filter screen and the railing on the inner liner member, the residual liquid in the inner liner member will flow out quickly, preventing the residual liquid from affecting the purity of diiodosilane. Then, the disc member drives the inner liner member to move upward, so that a plurality of connecting members contact the top of the sliding cavity, so that the four clamping posts no longer clamp with the four clamping members. At this time, the inner liner member falls onto the two limiting members. Through the arrangement of the inclined surfaces on the two limiting members, the inner liner member slides, and through the arrangement of the slope and the notch, the inner liner member slides into the storage box for collection. And when the inner liner member falls, the solution other than the residual crystal in the inner liner member is thrown out by the vibration force during the falling, further ensuring the purity of diiodosilane. Then, the electric telescopic rod drives the disc member to move downward, so that a plurality of second spring telescopic members are released, so that a plurality of first spring telescopic members are released, driving a plurality of inclined blocks to reset, so as to facilitate the clamping with the next inner liner member. Description of the Drawings

[0026] To more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings required in the embodiments. Obviously, the drawings in the following description are only some embodiments described in the present invention. For those of ordinary skill in the art, other drawings can also be obtained based on these drawings.

[0027] Figure 1 One of the structural schematic diagrams provided by the embodiments of the present invention;

[0028] Figure 2 Another structural schematic diagram provided by the embodiments of the present invention;

[0029] Figure 3 One of the internal structural schematic diagrams provided by the embodiments of the present invention;

[0030] Figure 4 Another internal structural schematic diagram provided by the embodiments of the present invention;

[0031] Figure 5 One of the partial structural schematic diagrams provided by the embodiments of the present invention;

[0032] Figure 6 Another partial structural schematic diagram provided by the embodiments of the present invention.

[0033] Explanation of reference numerals:

[0034] 1. Installation shell; 11. Sliding groove; 12. Sliding cavity; 13. Notch; 14. Ramp; 15. Storage box; 2. Driving assembly; 21. Electric telescopic rod; 22. Disc member; 23. Clamping post; 24. First spring telescopic member; 25. Inclined block; 26. Second spring telescopic member; 27. Connecting member; 28. First wire; 29. Limiting block; 3. Inner liner member; 31. Filter screen; 32. Rail; 33. Clamping member; 4. Limiting assembly; 41. Limiting unit; 411. Third spring telescopic member; 412. Limiting member; 413. Second wire; 42. Pressing block; 43. Fourth spring telescopic member. Detailed implementation manners

[0035] To enable those skilled in the art to better understand the technical solutions of the present invention, the following will further introduce the present invention in detail in conjunction with the drawings.

[0036] Please refer to Figures 1-6 , a purification method and purification processing system for disilane iodide provided by the embodiments of the present invention, and the following steps are carried out:

[0037] S1. Collect the crude disilane iodide liquid;

[0038] S2. Distill the crude disilane iodide liquid. The boiling point of disilane iodide is about 210°C;

[0039] S3. Collect the fraction after condensation to remove low-boiling impurities;

[0040] S4. Perform freeze crystallization on the distilled fraction. The freezing point of disilane diiodide is about -57°C;

[0041] S5. Filter to obtain crystals to remove high-boiling impurities;

[0042] S6. Add a reagent that can react with impurities and does not affect disilane diiodide;

[0043] S7. Perform distillation and filtration separation to remove residual impurities.

[0044] Preferably, it includes an installation shell 1. A driving component 2 is arranged on the installation shell 1. A liner part 3 is clamped on the output end of the driving component 2. The driving component 2 is slidably connected with a sliding groove 11 opened on the installation shell 1. The liner part 3 is located in a sliding cavity 12 inside the installation shell 1. The sliding cavity 12 communicates with the sliding groove 11. The sliding cavity 12 can collect the fraction in S4 and can withstand freezing to crystallize the fraction;

[0045] A limiting component 4 is installed on the installation shell 1. A notch 13 is opened on the installation shell 1. The inclined direction of the limiting component faces the notch.

[0046] Preferably, the driving component 2 includes an electric telescopic rod 21 arranged on the installation shell 1. The output end of the electric telescopic rod 21 is rotatably connected with a disc part 22. The disc part 22 is penetrated and fixedly connected by four clamping columns 23. Two first spring telescopic parts 24 are arranged on each of the four clamping columns 23. An inclined block 25 is arranged on the output end of each of the several first spring telescopic parts 24. Through the cooperation of the first spring telescopic parts 24 and the inclined blocks 25, the driving component 2 can be clamped and unclamped with the liner part 3, facilitating the limitation and collection of the liner part 3.

[0047] Preferably, two second spring telescopic parts 26 are fixed on each of the four clamping columns 23. A connecting part 27 is arranged on the output end of each of the several second spring telescopic parts 26. The several connecting parts 27 are respectively fixedly connected with one end of several first wires 28. The other ends of the several first wires 28 are respectively connected with several inclined blocks 25. When the several connecting parts 27 move up to contact the top of the sliding cavity 12, the several second spring telescopic parts 26 contract, driving the several inclined blocks 25 to be pulled, so that the driving component 2 can be unclamped from the liner part 3, enabling the liner part 3 to fall off. The solution other than the residual crystals in the liner part 3 is thrown out by the vibration force during the falling process, further ensuring the purity of disilane diiodide.

[0048] Preferably, the driving component 2 further includes a limiting block 29 fixedly arranged on the disc member 22. The limiting block 29 is slidably connected in the sliding groove 11. Through the cooperation of the limiting block 29 and the limiting groove, when the inner container member 3 moves upward, it can rotate first, so that the crystal no longer adheres to the sliding cavity 12, and the crystal can be taken out quickly.

[0049] Preferably, the bottom of the inner container member 3 is provided as a filter screen 31, the side of the inner container member 3 is provided with a plurality of railings 32, and four clamping members 33 are arranged on the inner container member 3. Four clamping grooves are respectively and correspondingly opened on the four clamping members 33, and the four clamping grooves respectively and correspondingly correspond to the positions of the four clamping columns 23. Through the arrangement of the four clamping grooves, the driving component 2 can be clamped with the inner container member 3.

[0050] Preferably, the limiting component 4 includes two limiting units 41. The limiting unit 41 includes two third spring telescopic members 411 fixedly arranged in the installation shell 1. A limiting member 412 is arranged at the output ends of the two third spring telescopic members 411. The limiting member 412 penetrates into the sliding cavity 12. An inclined surface is arranged on the limiting member 412, and the inclined direction of the inclined surface faces the notch 13. The limiting member 412 is fixedly connected to one end of a second wire 413. Through the cooperation between the third spring telescopic member 411 and the limiting member 412, the upward movement of the inner container member 3 will not be blocked, but the downward movement of the inner container member 3 will cause the inner container member 3 to slide out of the outside of the installation shell 1 through the arrangement of the inclined surface, so that the inner container member 3 can be collected.

[0051] Preferably, the two ends of the second wire 413 far from the limiting member 412 are fixedly connected to a pressing block 42. The pressing block 42 is fixedly arranged at the output end of a fourth spring telescopic member 43. The fourth spring telescopic member 43 is fixedly arranged on the installation shell 1. Through the cooperation of the pressing block 42 and the second wire 413, pressing the pressing block 42 can make the limiting member 412 withdraw from the sliding cavity 12, so that the arrangement of the limiting member 412 will not affect the next placement of the inner container member 3.

[0052] Preferably, a slope 14 is arranged on the installation shell 1. The slope 14 is connected to the two inclined surfaces. The slope 14 is located at the sliding groove 11. A storage box 15 is arranged on the installation shell 1. The storage box 15 corresponds to the position of the sliding groove 11. Through the arrangement of the slope 14, it can be ensured that the inner container member 3 enters the storage box 15 to ensure that the inner container member 3 can be collected.

[0053] Preferably, each bottom surface of the two limiting members 412 is provided with an inclined surface. Through the arrangement of the inclined surface, when the inner container member 3 moves upward, the two limiting members 412 can be pushed open, so that the two limiting members 412 will not affect the upward movement of the inner container member 3.

[0054] Working principle: By placing the inner container part 3 below the disc part 22, the four clamping grooves are respectively corresponding to the positions of the four clamping posts 23. Then, the inner container part 3 is lifted upward, so that several inclined blocks 25 are respectively in contact with the four clamping grooves, causing several first spring telescopic members 24 to contract, driving several inclined blocks 25 to be respectively retracted into the four clamping posts 23. When the inner container part 3 is lifted upward until it is no longer in contact with the inclined blocks 25, the four first spring telescopic members 24 are released, driving the four inclined blocks 25 to be released, so that the four clamping members 33 are respectively clamped with the four clamping posts 23 one by one;

[0055] Inject the diiodosilane solution to be purified into the sliding cavity 12. Then, start the electric telescopic rod 21 to drive the disc part 22 to move downward, so that the limiting block 29 moves downward. Through the setting of the sliding groove 11, the movement of the limiting block 29 is limited, so that the disc part 22 rotates after falling to a certain position, driving several clamping posts 23 to rotate, causing the inner container part 3 to rotate until the inner container part 3 falls to the bottom side position inside the sliding cavity 12. At the same time, sealant rings are arranged on the four sides of the disc part 22, so that the diiodosilane solution to be purified is sealed. Then, the diiodosilane solution to be purified is crystallized, and the crystallized diiodosilane will adhere to the inside of the sliding cavity 12;

[0056] Before moving downward, press the pressing block 42, so that the fourth spring telescopic member 43 contracts, driving the two second wires 413 to be pulled, so that the two limiting members 412 are pulled, so that the presence of the limiting members 412 will not affect the downward movement of the inner container part 3;

[0057] Start the electric telescopic rod 21 to drive the disc member 22 to move upward, so that the limit block 29 moves upward. Due to the setting of the sliding groove 11, the limit block 29 rotates when moving upward, driving the disc member 22 to rotate, causing the four clamping columns 23 to rotate, driving the inner liner member 3 to rotate, so that the disilane iodide crystal no longer adheres to the inner liner of the sliding cavity 12, and the crystal is located within the inner liner member 3. Then, the disc member 22 drives the inner liner member 3 to move upward, causing the disc member 22 to contact the inclined surfaces of the two limiting members 412, driving the two third spring telescopic members 411 to contract, so that the two limiting members 412 contract and withdraw from the sliding cavity 12. When the disc member 22 moves upward until the inner liner member 3 no longer contacts the two limiting members 412, the two third spring telescopic members 411 are released, driving the two limiting members 412 to reset. Then, the disc member 22 moves upward to drive the four clamping columns 23 to move upward, causing several second spring telescopic members 26 to move upward, driving several connecting members 27 to move upward, so that several connecting members 27 contact the top of the sliding cavity 12, driving several second spring telescopic members 26 to contract, pulling several first wires 28, driving several inclined blocks 25 to be pulled, causing several first spring telescopic members 24 to contract, so that the four clamping columns 23 no longer engage with the four clamping members 33. At this time, the inner liner member 3 drops onto the two limiting members 412. Due to the setting of the upper inclined surfaces of the two limiting members 412, the inner liner member 3 slides, and through the setting of the slope 14 and the notch 13, the inner liner member 3 slides into the storage box 15 for collection. Then, the electric telescopic rod 21 drives the disc member 22 to move downward, causing several second spring telescopic members 26 to be released, causing several first spring telescopic members 24 to be released, driving several inclined blocks 25 to reset, to facilitate engagement with the next inner liner member 3. Only some exemplary embodiments of the present invention have been described by way of illustration above. Undoubtedly, for those of ordinary skill in the art, without departing from the spirit and scope of the present invention, the described embodiments can be modified in various different ways. Therefore, the above drawings and description are illustrative in nature and should not be construed as limiting the scope of protection of the claims of the present invention.

Claims

1. A method for purifying diiodosilane, characterized in that: Follow these steps: S1. Collecting crude diiodosilane liquid; S2, distilling the crude diiodosilane liquid, the boiling point of diiodosilane is about 210°C; S3, collecting the condensed fraction to remove low-boiling impurities; S4, freeze-crystallize the distilled fraction, the freezing point of diiodosilane is about -57°C; S5, filtering to obtain crystals to remove high boiling point impurities; S6, adding a reagent that can react with the impurities and does not affect diiodosilane; S7. Perform distillation and filtration separation to remove residual impurities.

2. A diiodosilane purification processing system is used to implement a diiodosilane purification method according to claim 1, characterized in that: The invention comprises a mounting shell (1), a driving assembly (2) being arranged on the mounting shell (1), an inner liner (3) being clamped on the output end of the driving assembly (2), the driving assembly (2) being slidably connected to a sliding groove (11) provided on the mounting shell (1), the inner liner (3) being located in a sliding cavity (12) in the mounting shell (1), the sliding cavity (12) being connected to the sliding groove (11), the sliding cavity (12) being capable of collecting the fraction in S4 and being capable of withstanding freezing to crystallize the fraction; A limit assembly (4) is mounted on the mounting shell (1), a notch (13) is provided on the mounting shell (1), and the limit assembly is tilted toward the notch.

3. A diiodosilane purification processing system according to claim 2, characterized in that: The driving assembly (2) comprises an electric telescopic rod (21) arranged on the mounting shell (1); the output end of the electric telescopic rod (21) is rotatably connected to a disc member (22); the disc member (22) is penetrated by four clamping columns (23) and fixedly connected; two first spring telescopic members (24) are respectively arranged on the four clamping columns (23); and a plurality of the first spring telescopic members (24) are respectively arranged on their output ends with an inclined block (25).

4. A diiodosilane purification processing system according to claim 3, characterized in that: Two second spring telescopic members (26) are fixed on each of the four clamping columns (23); a connecting member (27) is provided on each output end of a plurality of the second spring telescopic members (26); the plurality of connecting members (27) are fixedly connected to one end of a plurality of first conducting wires (28) in a one-to-one correspondence; and the other ends of the plurality of first conducting wires (28) are connected to a plurality of inclined blocks (25) in a one-to-one correspondence.

5. A diiodosilane purification processing system according to claim 4, characterized in that: The driving assembly (2) further comprises a limit block (29) fixedly arranged on the disc member (22), wherein the limit block (29) is slidably connected in the sliding groove (11).

6. A diiodosilane purification processing system according to claim 5, characterized in that: The bottom of the inner container (3) is provided with a filter screen (31), the side of the inner container (3) is provided with a plurality of railings (32), the inner container (3) is provided with four clamping parts (33), the four clamping parts (33) are respectively provided with four clamping grooves corresponding to each other, and the four clamping grooves respectively correspond to the positions of the four clamping columns (23).

7. A diiodosilane purification processing system according to claim 6, characterized in that: The limiting assembly (4) comprises two limiting units (41), the limiting units (41) comprising two third spring expansion members (411) fixedly arranged in the mounting shell (1), a limiting member (412) being arranged at the output end of the two third spring expansion members (411), the limiting member (412) penetrating into the sliding cavity (12), an inclined surface being arranged on the limiting member (412), the inclined surface being inclined in a direction toward the notch (13), and the limiting member (412) being fixedly connected to one end of a second wire (413).

8. A diiodosilane purification processing system according to claim 7, characterized in that: One end of the two second conductive wires (413) away from the limiting member (412) is fixedly connected to a pressing block (42), the pressing block (42) is fixedly arranged at the output end of a fourth spring telescopic member (43), and the fourth spring telescopic member (43) is fixedly arranged on the mounting shell (1).

9. A diiodosilane purification processing system according to claim 8, characterized in that: The mounting shell (1) is provided with a slope (14), the slope (14) is connected to the two inclined surfaces, the slope (14) is located at the sliding groove (11), and the mounting shell (1) is provided with a storage box (15), the storage box (15) corresponds to the position of the sliding groove (11).

10. A diiodosilane purification processing system according to claim 9, characterized in that: The bottom surfaces of the two limiting members (412) are each provided with an inclined surface.

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