Device and method for preparing high-purity diiodosilane

Abstract

The invention discloses a preparation device and method of high-purity diiodosilane, and relates to the technical field of filter material preparation, the preparation device comprises a reaction kettle body and a cover plate fixedly mounted on the reaction kettle body, a servo motor is fixedly mounted on the cover plate, a stirring rod extending into the reaction kettle body is fixedly mounted at the output end of the servo motor, and the stirring rod is fixedly mounted on the reaction kettle body. The inner frame is fixedly mounted on the inner wall of the reaction kettle body, and a circular plate is fixedly mounted on the upper surface of the inner frame; the circular ring is fixedly mounted on the inner wall of the inner frame; and the first rotating rod and the second rotating rod are rotationally mounted on the circular plate. The stirring rod is controlled by the servo motor to rotate, materials can be ground at the same time, meanwhile, the materials can be located in an inert space and can immediately fall into the reaction kettle after being ground, so that the materials are prevented from being transferred after being ground, meanwhile, the grinding piece can conduct rotary and extrusion type grinding during grinding, and the grinding efficiency is improved. And therefore, the grinding effect is better.

Description

Technical Field

[0001] The invention relates to the technical field of filter material preparation, and in particular to a device and method for preparing high-purity diiodosilane. Background Art

[0002] Diiodosilane (DIS) is an advanced silicon-based precursor material with a wide range of uses, especially in the fields of materials science and chemistry. It can be vapor deposited on a variety of substrates, including crystalline silicon, polycrystalline silicon, amorphous silicon, organosilicon glass, fluorosilicone glass, organic polymer substrates, metal layers, and epitaxial fragmented silicon layers;

[0003] The application of diiodosilane in the manufacture of filter materials is mainly reflected in its role as a key material in the plasma enhanced atomic layer deposition (PEALD) process of silicon nitride films. In the PEALD process, diiodosilane, as a silicon source for deposition, can produce more active silicon radicals under plasma enhancement, which not only maintains a high deposition rate and carbon-free requirements, but also allows the deposition process to be carried out at a lower temperature and pressure, thereby improving the quality and performance of the film. Therefore, diiodosilane is often used to manufacture industrial dust removal filter materials;

[0004] For example, the invention patent with publication number CN110606491B and titled "A method for preparing high-purity diiodosilane" includes the following steps: under the protection of inert gas, with ether as solvent, react lithium aluminum tetrahydride and phenyldichlorosilane to obtain a phenylsilane mixture; heat the phenylsilane mixture, evaporate the phenylsilane, and collect the phenylsilane; control the reaction temperature to -80 to 30°C, add the collected phenylsilane dropwise to the powdered iodine element under stirring conditions, and add an oxygen-containing organic compound as a catalyst to obtain a diiodosilane mixture after the reaction; increase the temperature of the diiodosilane mixture to distill crude diiodosilane. The preparation method of high-purity diiodosilane proposed by the present invention uses non-toxic phenyldichlorosilane as the initial raw material, which greatly improves the safety of the process compared with the traditional initial raw material, the highly toxic chemical phenyltrichlorosilane.

[0005] In the process of manufacturing diiodosilane, a reactor is usually required to carry out a mixing reaction. The existing method for preparing diiodosilane is as shown in the above-mentioned patent, which comprises first preparing phenylsilane, then grinding iodine in an inert gas environment, and after the iodine is ground, adding phenylsilane dropwise into the iodine to react. However, the existing preparation equipment usually needs to operate the above method separately, and the iodine needs to be ground in a grinding device filled with inert gas first, and then poured into the reactor and phenylsilane is added dropwise to react. At the same time, the addition of phenylsilane also needs to be controlled separately, so that the experimenter needs to perform multiple rounds of operations during the entire experiment, making the preparation experiment cumbersome and complicated. Summary of the invention

[0006] The object of the present invention is to provide a device and method for preparing high-purity diiodosilane to solve the above-mentioned deficiencies in the prior art.

[0007] In order to achieve the above-mentioned purpose, the present invention provides the following technical solutions: a preparation device for high-purity diiodosilane, comprising a reactor body and a cover plate fixedly mounted thereon, a servo motor fixedly mounted on the cover plate, a stirring rod extending into the reactor body fixedly mounted on the output end of the servo motor, and further comprising: an inner frame fixedly mounted on the inner wall of the reactor body, a circular plate fixedly mounted on the upper surface of the inner frame; a circular ring fixedly mounted on the inner wall of the inner frame; a first rotating rod and a second rotating rod, both of which are rotatably mounted on the circular plate; a first belt, which is transmission-mounted between the first rotating rod and the stirring rod; a third rotating rod, which is arranged in the circular ring, and a grinding piece is fixedly mounted on the bottom end of the third rotating rod; while the stirring rod is stirring, the first belt will drive the first rotating rod to rotate synchronously, and at this time the first rotating rod will drive the third rotating rod to rotate and move up and down through the second rotating rod, so that the grinding piece rotates and presses the material in the circular ring for grinding.

[0008] Preferably, a protrusion is fixedly mounted on the bottom end of the first rotating rod, a connecting block is slidably mounted on the second rotating rod, and both the protrusion and the connecting block are provided with inclined surfaces, and a gap is provided between the first rotating rod and the second rotating rod.

[0009] Preferably, a square rod is vertically slidably installed inside the second rotating rod, and the square rod is fixedly connected to the top end of the third rotating rod, and a first spring is fixedly installed between the top end of the square rod and the inner top wall of the second rotating rod;

[0010] A round ball is fixedly mounted on the top end of the third rotating rod, a round disc is fixedly mounted on the bottom end of the round plate, and a square plate is fixedly mounted on the bottom end of the round disc.

[0011] Preferably, a grinding groove is provided in the ring;

[0012] The grinding piece and the grinding groove are both in a truncated cone shape.

[0013] Preferably, a blocking block is slidably installed at the bottom end of the circular ring, a connecting plate is fixedly installed at the bottom end of the blocking block, a vertical pole is fixedly installed on the connecting plate, a screw is threadedly inserted on the vertical pole, a rotating shaft is rotatably installed on the circular plate, a friction disk is fixedly installed on the rotating shaft, the friction disk and the first rotating rod are in fit shape, and a second belt is installed for transmission between the top end of the rotating shaft and the screw.

[0014] Preferably, a limit frame is fixedly mounted on the bottom end of the inner frame, and the limit frame is in a "concave" shape.

[0015] Preferably, a slip ring is sleeved on the surface of the second rotating rod, an abutment rod is fixedly installed on the bottom end of the slip ring, a long plate is slidably installed on the circular plate, a liquid inlet pipe is fixedly installed on the cover plate, the long plate is inserted into the interior of the liquid inlet pipe, and a through hole is opened on the surface of the long plate, chamfers are provided between the long plate and the abutment rod, and the connecting block is L-shaped.

[0016] Preferably, an outer frame is fixedly mounted on the circular plate, a top plate is fixedly mounted on the long plate, and a second spring is fixedly mounted between the top plate and the outer frame.

[0017] Preferably, a limit strip is fixedly mounted on the bottom end of the slip ring.

[0018] A method for preparing high-purity diiodosilane, using the preparation device described in any one of the above, comprises the following steps:

[0019] S1. Clean the reactor and its liquid inlet pipe and feed pipe;

[0020] S2, placing the grinding material into the grinding groove of the ring;

[0021] S3, connecting the liquid inlet pipe to the container of the solution;

[0022] S4, introducing inert gas into the inner frame through the hose and the feed pipe;

[0023] S5, start the servo motor to drive the stirring rod to rotate forward so that the grinding element grinds the material;

[0024] S6. Control the servo motor to reverse so that it drives the block to open and put down the ground material, and at the same time drip in the phenylsilane solution.

[0025] In the above technical scheme, the present invention provides a device and method for preparing high-purity diiodosilane, which has the following beneficial effects: the present application can grind the material at the same time by controlling the rotation of the stirring rod through a servo motor, and the material can be in an inert space and can fall into the reactor immediately after grinding, thereby avoiding the transfer of the material after grinding. At the same time, during grinding, the grinding piece can be rotated and extruded to grind, thereby achieving a better grinding effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For ordinary technicians in this field, other drawings can also be obtained based on these drawings.

[0027] Figure 1 A schematic diagram of a three-dimensional structure provided by an embodiment of the present invention;

[0028] Figure 2 A schematic diagram of the internal structure of a reactor provided in an embodiment of the present invention;

[0029] Figure 3 The embodiment of the present invention provides Figure 2 Schematic diagram of the bottom structure;

[0030] Figure 4 The embodiment of the present invention provides Figure 2 Schematic diagram of the internal structure;

[0031] Figure 5-7 All of them are partial structural schematic diagrams of the inner ring provided by the embodiments of the present invention;

[0032] Figure 8 A partial structural schematic diagram of a long board provided in an embodiment of the present invention.

[0033] Description of reference numerals:

[0034] 1. Reactor body; 2. Servo motor; 3. Cover plate; 4. Liquid inlet pipe; 5. Feed pipe; 6. Inner frame; 71. First belt; 72. First rotating rod; 73. Second rotating rod; 74. Bump; 75. Connecting block; 76. Disc; 77. Square plate; 78. Third rotating rod; 79. Ball; 710. Ring; 711. Grinding piece; 712. Grinding groove; 81. Block; 82. Connecting plate; 83. Vertical rod; 84. Screw; 85. Second belt; 86. Friction disc; 87. Rotating shaft; 88. Limiting frame; 91. Slip ring; 92. Abutting rod; 93. Long plate; 94. Limiting strip; 95. Outer frame; 96. Top plate. DETAILED DESCRIPTION

[0035] In order to enable those skilled in the art to better understand the technical solution of the present invention, the present invention will be further described in detail below with reference to the accompanying drawings.

[0036] See also Figure 1-8 A device and method for preparing high-purity diiodosilane, comprising a reactor body 1 and a cover plate 3 fixedly mounted thereon, a servo motor 2 fixedly mounted on the cover plate 3, a stirring rod extending into the reactor body 1 fixedly mounted at the output end of the servo motor 2, and further comprising:

[0037] An inner frame 6 is fixedly mounted on the inner wall of the reactor body 1, and a circular plate is fixedly mounted on the upper surface of the inner frame 6;

[0038] A circular ring 710, which is fixedly mounted on the inner wall of the inner frame 6;

[0039] A first rotating rod 72 and a second rotating rod 73, both of which are rotatably mounted on the circular plate;

[0040] A first belt 71, which is installed between the first rotating rod 72 and the stirring rod;

[0041] A third rotating rod 78 is disposed in the ring 710, and a grinding member 711 is fixedly mounted on the bottom end of the third rotating rod 78;

[0042] While the stirring rod is stirring, the first belt 71 will drive the first rotating rod 72 to rotate synchronously, and at this time, the first rotating rod 72 will drive the third rotating rod 78 to rotate and move up and down through the second rotating rod 73, so that the grinding member 711 rotates and presses the material in the ring 710 to grind;

[0043] A fixing ring is fixedly mounted on the circular plate, and the first rotating rod 72 is rotatably mounted in the fixing ring, so as to ensure the rotation of the first rotating rod 72 .

[0044] In another embodiment of the present invention: a protrusion 74 is fixedly installed at the bottom end of the first rotating rod 72, a connecting block 75 is slidably installed on the second rotating rod 73, and both the protrusion 74 and the connecting block 75 are provided with inclined surfaces, and a gap is provided between the first rotating rod 72 and the second rotating rod 73;

[0045] When the stirring rod rotates forward, the stirring rod will drive the first rotating rod 72 to rotate through the first belt 71. At this time, the vertical end of the protrusion 74 will contact the vertical end of the connecting block 75. At this time, the rotation of the first rotating rod 72 will drive the second rotating rod 73 to rotate synchronously through the protrusion 74 and the connecting block 75. When the stirring rod is reversed, the inclined surface of the protrusion 74 on the first rotating rod 72 will contact the inclined surface on the connecting block 75. At this time, since the protrusion 74 will not move up and down, as the protrusion 74 squeezes the connecting block 75, the connecting block 75 will move downward in the second rotating rod 73, so that the rotation of the first rotating rod 72 will not cause the second rotating rod 73 to rotate.

[0046] In another embodiment of the present invention: a square rod is vertically slidably installed inside the second rotating rod 73, and the square rod is fixedly connected to the top end of the third rotating rod 78, and a first spring is fixedly installed between the top end of the square rod and the inner top wall of the second rotating rod 73;

[0047] A round ball 79 is fixedly mounted on the top of the third rotating rod 78, a round disc 76 is fixedly mounted on the bottom of the round plate, and a square plate 77 is fixedly mounted on the bottom of the round disc 76;

[0048] When the second rotating rod 73 rotates, it will drive the third rotating rod 78 to rotate through the square rod. At the same time, since the square rod can move vertically in the second rotating rod 73, when the third rotating rod 78 rotates, the ball 79 thereon contacts the square plate 77, the square plate 77 will squeeze the ball 79 so that the third rotating rod 78 with the ball 79 moves downward. At this time, the third rotating rod 78 will drive the square rod to move downward, and the first spring will be stretched. As the ball 79 moves away from the square plate 77, the first spring will pull the square rod to rise and reset.

[0049] In another embodiment of the present invention: a grinding groove 712 is provided in the ring 710;

[0050] The grinding member 711 and the grinding groove 712 are both in the shape of a truncated cone;

[0051] When the third rotating rod 78 rotates following the second rotating rod 73, the grinding member 711 will rotate in the grinding groove 712 to grind the material in the grinding groove 712. At the same time, when the square rod moves downward, the grinding member 711 will move downward to squeeze the material in the grinding groove 712, thereby achieving a better grinding effect.

[0052] In another embodiment of the present invention: a block 81 is slidably mounted on the bottom end of the circular ring 710, a connecting plate 82 is fixedly mounted on the bottom end of the block 81, a vertical rod 83 is fixedly mounted on the connecting plate 82, a screw 84 is threadedly inserted on the vertical rod 83, a rotating shaft 87 is rotatably mounted on the circular plate, a friction disk 86 is fixedly mounted on the rotating shaft 87, the friction disk 86 and the first rotating rod 72 are fitted, and a second belt 85 is installed between the top end of the rotating shaft 87 and the screw 84 for transmission;

[0053] When the stirring rod rotates forward, it will drive the grinding piece 711 to grind. At this time, the block 81 is located inside the ring 710 and the inner frame 6, and the connecting plate 82 will abut against the bottom end of the inner frame 6. At this time, due to the restriction of the connecting plate 82 and the vertical rod 83, the screw 84 will not rotate, so that the friction plate 86 cannot rotate. At this time, the contact between the first rotating rod 72 and the friction plate 86 will not drive the friction plate 86 to rotate. When the stirring rod is reversed, the first rotating rod 72 will also be reversed. At this time, the first rotating rod 72 will drive the friction plate 86 to rotate. At the same time, the friction plate 86 will drive the rotating shaft 87 to rotate and drive the screw 84 to rotate through the second belt 85. At this time, the screw 84 will drive the vertical rod 83 to descend. At this time, the descent of the vertical rod 83 will drive the connecting plate 82 to move downward, so that the block 81 is moved out. At this time, the bottom of the ring 710 and the inner frame 6 will be opened, so that the ground material falls into the interior of the reactor.

[0054] In another embodiment of the present invention: a limit frame 88 is fixedly installed at the bottom end of the inner frame 6, and the limit frame 88 is in a "concave" shape;

[0055] When the first rotating rod 72 continues to rotate and drives the vertical rod 83 to descend through the screw rod 84 until the connecting plate 82 contacts the limit frame 88, the limit frame 88 will limit the downward movement of the connecting plate 82. At this time, the screw rod 84 will no longer be able to rotate, and at the same time, the rotation of the first rotating rod 72 will not drive the friction plate 86 to rotate. However, since the friction plate 86 and the first rotating rod 72 are in contact with each other, the friction plate 86 will not affect the rotation of the first rotating rod 72.

[0056] In another embodiment of the present invention: a slip ring 91 is sleeved on the surface of the second rotating rod 73, an abutting rod 92 is fixedly installed on the bottom end of the slip ring 91, a long plate 93 is slidably installed on the circular plate, a liquid inlet pipe 4 is fixedly installed on the cover plate 3, the long plate 93 is inserted into the inside of the liquid inlet pipe 4, and a through hole is opened on the surface of the long plate 93, chamfers are provided between the long plate 93 and the abutting rod 92, and the connecting block 75 is L-shaped;

[0057] When the first rotating rod 72 rotates forward to drive the second rotating rod 73 to rotate for grinding, the connecting block 75 will not move downward at this time, so that the connecting block 75 slides on the surface of the slip ring 91, and when the first rotating rod 72 is reversed, the ground material will fall off, and the protrusion 74 will also squeeze the connecting block 75 to move downward. At this time, since the connecting block 75 is L-shaped, the short wall end of the L-shaped connecting block 75 extends from the surface of the second rotating rod 73. At this time, as the connecting block 75 moves downward, it will push the slip ring 91 to move downward, and as the first rotating rod 72 is reversed, the ground material will fall off, and the protrusion 74 will also squeeze the connecting block 75 to move downward. As the sliding ring 91 moves downward, it will drive the abutting rod 92 to move downward. At this time, the abutting rod 92 will push the long plate 93 to move through the chamfers on it and the long plate 93. At this time, the long plate 93 will slide in the liquid inlet pipe 4, wherein the through hole on the long plate 93 is staggered with the liquid inlet port of the liquid inlet pipe 4 in the initial state, so that the liquid in the liquid inlet pipe 4 will not enter the reactor. When the abutting rod 92 pushes the long plate 93 to slide, the through hole slides to align with the liquid inlet port, so that the liquid in the liquid inlet pipe 4 flows into the reactor;

[0058] A feed pipe 5 is provided on the cover plate 3, and the feed pipe 5 passes through the inner frame 6, wherein the surface of the feed pipe 5 begins to have side holes, and the side holes are located in the inner frame 6, wherein the grinding of iodine element usually needs to be carried out under inert gas, at this time, a hose can be introduced into the feed pipe 5, so that the hose is connected to the side hole, and the inert gas can be introduced into the inner frame 6 through the hose, so that the grinding is in the inert gas, and with the end of grinding, when the iodine element is added to the reactor, it is often necessary to add phenylsilane, at this time, with the reverse rotation of the first rotating rod 72, it continuously presses the connecting block 75 through the protrusion 74, so that the connecting block 75 moves back and forth up and down, so that the long plate 93 moves repeatedly in the liquid inlet pipe 4, so that the through hole on the long plate 93 slowly adds phenylsilane.

[0059] In another embodiment of the present invention: an outer frame 95 is fixedly mounted on the circular plate, a top plate 96 is fixedly mounted on the long plate 93, and a second spring is fixedly mounted between the top plate 96 and the outer frame 95;

[0060] When the abutment rod 92 squeezes the long plate 93 to move the long plate 93 toward the liquid inlet pipe 4, as the connecting block 75 rises, the abutment rod 92 will also rise, and at this time the second spring will pull the top plate 96 to move, so that the top plate 96 drives the long plate 93 to slide and return to its original position in the liquid inlet pipe 4.

[0061] In another embodiment of the present invention: a limit strip 94 is fixedly installed at the bottom end of the slip ring 91;

[0062] There are multiple limit bars 94, and the limit bars 94 are inserted in the circular plate. At the same time, a return spring is fixedly installed at the bottom end of the limit bar 94. The limit bar 94 can limit the movement of the slip ring 91, thereby preventing the slip ring 91 from rotating. At the same time, the return spring can push the slip ring 91 to rise when the connecting block 75 rises.

[0063] A method for preparing high-purity diiodosilane, using any of the above preparation devices, comprises the following steps:

[0064] S1. Clean the reactor and the liquid inlet pipe 4 and the feed pipe 5 thereon;

[0065] S2, placing the grinding material into the grinding groove 712 of the ring 710;

[0066] S3, connecting the liquid inlet pipe 4 with the container of the solution;

[0067] S4, introducing inert gas into the inner frame 6 through the hose and the feed pipe 5;

[0068] S5, start the servo motor 2 to first drive the stirring rod to rotate forward so that the grinding element 711 grinds the material;

[0069] S6, controlling the servo motor 2 to reverse so that it drives the block 81 to open and put down the ground material, and at the same time dripping the phenylsilane solution.

[0070] The above description is only by way of illustration of certain exemplary embodiments of the present invention. It is undoubted that those skilled in the art can modify the described embodiments in various ways without departing from the spirit and scope of the present invention. Therefore, the above drawings and descriptions 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 device for preparing high-purity diiodosilane, comprising a reactor body (1) and a cover plate (3) fixedly mounted thereon, a servo motor (2) fixedly mounted on the cover plate (3), a stirring rod extending into the reactor body (1) fixedly mounted at the output end of the servo motor (2), characterized in that: Also includes: An inner frame (6) is fixedly mounted on the inner wall of the reactor body (1), and a circular plate is fixedly mounted on the upper surface of the inner frame (6); A circular ring (710) fixedly mounted on the inner wall of the inner frame (6); A first rotating rod (72) and a second rotating rod (73), both of which are rotatably mounted on a circular plate; A first belt (71) is installed between the first rotating rod (72) and the stirring rod; A third rotating rod (78) is disposed in the circular ring (710), and a grinding member (711) is fixedly mounted on the bottom end of the third rotating rod (78); While the stirring rod is stirring, the first belt (71) will drive the first rotating rod (72) to rotate synchronously. At this time, the first rotating rod (72) will drive the third rotating rod (78) to rotate and move up and down through the second rotating rod (73), so that the grinding member (711) rotates and presses the material in the ring (710) to grind.

2. The preparation device of high-purity diiodosilane according to claim 1, characterized in that: A protrusion (74) is fixedly mounted on the bottom end of the first rotating rod (72), a connecting block (75) is slidably mounted on the second rotating rod (73), and both the protrusion (74) and the connecting block (75) are provided with inclined surfaces, and a gap is provided between the first rotating rod (72) and the second rotating rod (73).

3. The preparation device of high-purity diiodosilane according to claim 2, characterized in that: A square rod is vertically slidably mounted inside the second rotating rod (73), and the square rod is fixedly connected to the top end of the third rotating rod (78), and a first spring is fixedly mounted between the top end of the square rod and the inner top wall of the second rotating rod (73); A round ball (79) is fixedly mounted on the top end of the third rotating rod (78), a round disc (76) is fixedly mounted on the bottom end of the round plate, and a square plate (77) is fixedly mounted on the bottom end of the round disc (76).

4. The preparation device of high-purity diiodosilane according to claim 1, characterized in that: A grinding groove (712) is provided in the circular ring (710); The grinding piece (711) and the grinding groove (712) are both in the shape of a truncated cone.

5. The device for preparing high-purity diiodosilane according to claim 4, characterized in that: A blocking block (81) is slidably mounted on the bottom end of the circular ring (710), a connecting plate (82) is fixedly mounted on the bottom end of the blocking block (81), a vertical rod (83) is fixedly mounted on the connecting plate (82), a screw rod (84) is threadedly inserted on the vertical rod (83), a rotating shaft (87) is rotatably mounted on the circular plate, a friction disk (86) is fixedly mounted on the rotating shaft (87), the friction disk (86) and the first rotating rod (72) are in close contact, and a second belt (85) is installed between the top end of the rotating shaft (87) and the screw rod (84) for transmission.

6. The device for preparing high-purity diiodosilane according to claim 1, characterized in that: A limit frame (88) is fixedly mounted on the bottom end of the inner frame (6), and the limit frame (88) is in a concave shape.

7. The device for preparing high-purity diiodosilane according to claim 2, characterized in that: The surface of the second rotating rod (73) is sleeved with a slip ring (91), the bottom end of the slip ring (91) is fixedly mounted with an abutting rod (92), a long plate (93) is slidably mounted on the circular plate, a liquid inlet pipe (4) is fixedly mounted on the cover plate (3), the long plate (93) is inserted into the interior of the liquid inlet pipe (4), and a through hole is opened on the surface of the long plate (93), chamfers are provided between the long plate (93) and the abutting rod (92), and the connecting block (75) is L-shaped.

8. The device for preparing high-purity diiodosilane according to claim 7, characterized in that: An outer frame (95) is fixedly mounted on the circular plate, a top plate (96) is fixedly mounted on the long plate (93), and a second spring is fixedly mounted between the top plate (96) and the outer frame (95).

9. The device for preparing high-purity diiodosilane according to claim 7, characterized in that: A limit strip (94) is fixedly mounted on the bottom end of the slip ring (91).

10. A method for preparing high-purity diiodosilane, characterized in that: The preparation device according to any one of claims 1 to 9 comprises the following steps: S1. Clean the reactor and the liquid inlet pipe (4) and feed pipe (5) thereon; S2, placing the grinding material into the grinding groove (712) of the ring (710); S3, connecting the liquid inlet pipe (4) to the container of the solution; S4, introducing inert gas into the inner frame (6) through the hose and the feed pipe (5); S5, starting the servo motor (2) to first drive the stirring rod to rotate forward so that the grinding element (711) grinds the material; S6, controlling the servo motor (2) to reverse so that it drives the block (81) to open and place the ground material, and at the same time dripping the phenylsilane solution.

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