CN116119627A - High alpha phase silicon nitride powder synthesis method - Google Patents
High alpha phase silicon nitride powder synthesis method Download PDFInfo
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- CN116119627A CN116119627A CN202310089025.2A CN202310089025A CN116119627A CN 116119627 A CN116119627 A CN 116119627A CN 202310089025 A CN202310089025 A CN 202310089025A CN 116119627 A CN116119627 A CN 116119627A
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- 239000000843 powder Substances 0.000 title claims abstract description 51
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 49
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000001308 synthesis method Methods 0.000 title claims description 7
- 239000007788 liquid Substances 0.000 claims abstract description 57
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 30
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 229910003902 SiCl 4 Inorganic materials 0.000 claims abstract description 9
- 230000009471 action Effects 0.000 claims abstract description 8
- 238000005507 spraying Methods 0.000 claims abstract description 4
- 238000012216 screening Methods 0.000 claims description 32
- 238000003756 stirring Methods 0.000 claims description 28
- 238000003860 storage Methods 0.000 claims description 24
- 230000001681 protective effect Effects 0.000 claims description 16
- 230000005540 biological transmission Effects 0.000 claims description 15
- 238000005192 partition Methods 0.000 claims description 12
- 238000007599 discharging Methods 0.000 claims description 11
- 238000001802 infusion Methods 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 7
- 238000009423 ventilation Methods 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 238000010924 continuous production Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000005245 sintering Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- -1 silicon imine Chemical class 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/068—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with silicon
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Abstract
The invention relates to the technical field of inorganic nonmetallic materials, in particular to a method for synthesizing high alpha-phase silicon nitride powder, which comprises the following steps: step one: siCl is added to 4 NH (NH) 3 Mixing the liquid; step two: the SiCl obtained in the step one is treated 4 NH (NH) 3 Spraying the liquid mixture into a reaction cavity with a microwave magnetron through a nozzle, and SiCl 4 NH (NH) 3 The liquid mixture reacts by microwave action to produce alpha phase silicon nitride powder. The method can realize continuous production of the alpha-phase silicon nitride powder, and has higher yield and finer product powder. The method uses microwave heating, has low reaction temperature, improves the safety of the production process, has high alpha phase content of the generated product, and improves the quality of alpha phase silicon nitride powder; the invention has low production cost.
Description
Technical Field
The invention relates to the technical field of inorganic nonmetallic materials, in particular to a method for synthesizing high alpha-phase silicon nitride powder.
Background
The past research experience of silicon nitride ceramic sintering shows that the alpha-phase silicon nitride powder has better sintering activity, can improve the sintering density of the silicon nitride ceramic, and provides more excellent performance indexes. The alpha phase content in the current commercial silicon nitride powder is also one of the key technical indicators. The main synthesis methods of the existing silicon nitride powder synthesis include a direct nitridation method, a silicon imine decomposition method, a carbothermal reduction method and the like, and the existing synthesis method has high reaction temperature.
Disclosure of Invention
The invention aims to provide a method for synthesizing high alpha-phase silicon nitride powder, which reduces the reaction temperature by using microwave heating.
In order to solve the problems, the invention discloses a method for synthesizing high alpha-phase silicon nitride powder, which comprises the following steps:
step one: siCl is added to 4 NH (NH) 3 Mixing the liquid;
step two: the SiCl obtained in the step one is treated 4 NH (NH) 3 Spraying the liquid mixture into a reaction cavity with a microwave magnetron through a nozzle, and SiCl 4 NH (NH) 3 The liquid mixture reacts by microwave action to produce alpha phase silicon nitride powder.
Preferably, the first and second steps are performed based on a production apparatus including a synthesizing apparatus including:
the device comprises a shell, wherein a baffle plate is fixedly connected inside the shell, the interior of the shell is divided into a mixing cavity and a reaction cavity by the baffle plate, the reaction cavity is positioned below the mixing cavity, the lower end of the shell is connected with a fixed bracket, and the fixed bracket is fixedly connected with the upper end of a bottom plate;
the mixing tank is fixedly connected with the upper surface of the partition plate, two liquid inlets are symmetrically formed in the left and right of the upper end of the mixing tank, and a liquid outlet is formed in the lower end of the mixing tank;
the sprayer is fixedly connected to the lower surface of the partition board;
one end of the infusion tube is communicated with the liquid outlet, the other end of the infusion tube is communicated with the liquid inlet of the sprayer, and the infusion tube is connected with a first booster pump;
the discharging plate is fixedly connected to the lower side of the right wall of the reaction cavity, and a blanking valve is connected to the discharging plate;
the microwave magnetrons are uniformly distributed and connected to the inner wall of the reaction cavity.
Preferably, the synthesizing device further comprises two groups of bilaterally symmetrical raw material input groups, and the two groups of bilaterally symmetrical raw material input groups are respectively used for inputting liquid to the two liquid inlets.
Preferably, the raw material input group includes:
the storage tank is fixedly connected to the left side or the right side of the upper surface of the partition plate;
the liquid inlet funnel is fixedly connected with a liquid inlet pipe at the lower end, and the liquid inlet pipe penetrates through the shell and is inserted into the storage tank;
the transmission pipeline, transmission pipeline one end and holding vessel intercommunication, the transmission pipeline other end is connected in the feed liquor mouth that corresponds with the connection, be connected with force (forcing) pump two on the transmission pipeline.
Preferably, the mixing tank is also connected with a stirring assembly.
Preferably, the stirring assembly comprises: a motor case, a motor and a stirring rod;
the motor box is fixedly connected to the outer side of the upper end of the shell, and the motor is arranged in the motor box;
the upper end of the stirring rod is fixedly connected with an output shaft of the motor, and the stirring rod penetrates through the upper end of the mixing tank;
the stirring rod lower part fixedly connected with a plurality of stirring leaves, stirring leaves are located in the reaction cavity.
Preferably, the synthesizing device further comprises a controller, and the controller is electrically connected with the first pressurizing pump, the second pressurizing pump, the motor and the microwave magnetron.
Preferably, the apparatus further comprises a sorting apparatus disposed below the right side of the synthesizing apparatus, the sorting apparatus comprising:
the device comprises a box body, wherein a gas tank cavity and a screening cavity are arranged in the box body, a chute is formed in the inner wall of the screening cavity, a first opening is formed in the left side of the upper end of the box body, the first opening is positioned below a discharging plate, and the box body is fixedly connected to the upper end of a bottom plate;
the rotating shaft is rotationally connected with the right side of the first opening, and a gear is fixedly connected to the rotating shaft;
the protective cover is fixedly connected with the left end of the rotating shaft and is positioned above the screening cavity, and the protective cover is used for sealing or opening the first opening;
the rack bar is meshed with the gear for transmission, the top end of the rack bar is fixedly connected with a pressing plate, and the lower end of the rack bar is rotatably connected with a roller;
two magnetic blocks, one of which is fixedly connected to the lower surface of the pressing plate, and the other of which is fixedly connected to the upper surface of the box body;
the gas tank frame is fixedly connected with the inner wall of the gas tank cavity, and a gas storage tank is arranged on the gas tank frame;
the collecting box is connected in the chute in a sliding manner along the up-down direction, and the side wall of the collecting box is provided with a vent hole;
the conical block is connected with the inner wall of the screening cavity in a sliding manner along the left-right direction, and is positioned below the roller, and the roller is contacted with the conical surface of the conical block;
one end of the connecting rod is hinged with the conical block, and the other end of the connecting rod is hinged with the bottom of the collecting box;
the two mounting frames are fixedly connected with the inner walls of the left side and the right side of the collecting box respectively, and the upper surface of each mounting frame is fixedly connected with a fixing rod;
the cam is rotationally connected with the mounting frame through a rotating shaft in the front-rear direction, and a driving device is arranged on the mounting frame and used for driving the cam to rotate;
one end of the air pipe is communicated with the air storage tank, and the other end of the air pipe penetrates through the left side wall of the air storage tank cavity;
screening bucket, the left portion and the right part of screening bucket all set up the extension, and left portion and right part extension are respectively along upper and lower direction slip cup joint on corresponding dead lever, screening bucket lower surface opening, and screening bucket lower surface is provided with the screen cloth, and the extension lower extreme of left portion and right part contacts with corresponding cam respectively.
The beneficial effects of the invention are as follows: the invention uses SiCl 4 NH (NH) 3 The liquid mixture is sprayed into a reaction cavity through a nozzle, and the reaction cavity is provided with a microwave magnetron and SiCl 4 NH (NH) 3 The liquid mixture reacts by microwave action to produce alpha phase silicon nitride powder. The method can realize continuous production of the alpha-phase silicon nitride powder, and has higher yield and finer product powder. The method of the invention uses microwave heating, has low reaction temperature and improves the safety of the production processThe alpha phase content of the generated product is high, and the quality of alpha phase silicon nitride powder is improved; the invention has low production cost.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims thereof as well as the appended drawings.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention. In the drawings:
FIG. 1 is a flow chart of the synthetic method of the present invention;
FIG. 2 is a schematic view of the whole production device of the present invention;
FIG. 3 is a schematic diagram of the synthesis apparatus of the present invention;
FIG. 4 is a schematic diagram of the sorting apparatus of the present invention;
fig. 5 is a schematic view showing the connection state of the rotating rod and the gear in the sorting device according to the present invention.
In the figure: 1. a synthesizing device; 101. a housing; 1011. a mixing chamber; 1012. a reaction chamber; 2. a partition plate; 3. a mixing tank; 4. a liquid inlet; 5. a liquid outlet; 6. a sprayer; 7. an infusion tube; 8. a pressurizing pump I; 9. a microwave magnetron; 10. a storage tank; 11. a liquid inlet funnel; 12. a transmission pipeline; 13. a second pressurizing pump; 14. a motor case; 15. a motor; 16. a stirring rod; 17. stirring the leaves; 18. a sorting device; 181. a case; 1811. a gas tank chamber; 1812. a screening cavity; 1813. a chute; 1814. a first opening; 19. a rotating shaft; 20. a gear; 21. a protective cover; 22. a rack bar; 23. pressing the plate; 24. a roller; 25. a magnetic block; 26. a gas tank rack; 27. a gas storage tank; 28. a collection box; 29. a vent hole; 30. a conical block; 31. a connecting rod; 32. a mounting frame; 33. a fixed rod; 34. a cam; 35. a ventilation duct; 36. screening barrels; 37. a screen; 38. an extension; 39. a blanking valve; 40. a discharge plate; 41. a fixed bracket; 42. a bottom plate.
Detailed Description
The preferred embodiments of the present invention will be described below with reference to the accompanying drawings, it being understood that the preferred embodiments described herein are for illustration and explanation of the present invention only, and are not intended to limit the present invention. In addition, technical solutions and technical features between the embodiments may be combined with each other, but it is necessary to base that a person skilled in the art can implement the combination of technical solutions, when the combination of technical solutions contradicts or cannot be implemented, should be considered that the combination of technical solutions does not exist, and is not within the scope of protection claimed by the present invention.
Example 1: the embodiment of the invention provides a method for synthesizing high alpha-phase silicon nitride powder, which comprises the following steps:
step one: siCl is added to 4 NH (NH) 3 Mixing the liquid;
step two: the SiCl obtained in the step one is treated 4 NH (NH) 3 Spraying the liquid mixture into a reaction cavity with a microwave magnetron through a nozzle, and SiCl 4 NH (NH) 3 The liquid mixture reacts by microwave action to produce alpha phase silicon nitride powder.
The beneficial effects of the technical scheme are as follows: the invention uses SiCl 4 NH (NH) 3 The liquid mixture is sprayed into the reaction chamber 1012 through a nozzle, and the reaction chamber 1012 is provided with a microwave magnetron 9 and SiCl 4 NH (NH) 3 The liquid mixture reacts by microwave action to produce alpha phase silicon nitride powder. The method can realize continuous production of the alpha-phase silicon nitride powder, and has higher yield and finer product powder. The method uses microwave heating, has low reaction temperature, improves the safety of the production process, has high alpha phase content of the generated product, and improves the quality of alpha phase silicon nitride powder; the invention has low production cost.
Example 2: on the basis of the embodiment 1, as shown in fig. 1 and 2, the embodiment of the invention further provides a high alpha phase silicon nitride powder synthesis method, which is applied to the high alpha phase silicon nitride powder synthesis method, wherein the production device comprises a synthesis device 1, and the synthesis device 1 comprises:
the device comprises a shell 101, wherein a baffle plate 2 is fixedly connected inside the shell 101, the interior of the shell 101 is divided into a mixing cavity 1011 and a reaction cavity 1012 by the baffle plate 2, the reaction cavity 1012 is positioned below the mixing cavity 1011, the lower end of the shell 101 is connected with a fixed support 41, and the fixed support 41 is fixedly connected with the upper end of a bottom plate 42;
the mixing tank 3 is fixedly connected with the upper surface of the partition plate 2, two liquid inlets 4 are symmetrically formed in the left and right of the upper end of the mixing tank 3, and a liquid outlet 5 is formed in the lower end of the mixing tank 3;
the sprayer 6 is fixedly connected to the lower surface of the partition board 2;
one end of the infusion tube 7 is communicated with the liquid outlet 5, the other end of the infusion tube 7 is communicated with the liquid inlet of the sprayer 6, and the infusion tube 7 is connected with a first booster pump 8;
the discharging plate 40 is fixedly connected to the lower side of the right wall of the reaction cavity 1012, and the discharging plate 40 is connected with a blanking valve 39;
and the plurality of microwave magnetrons 9 are uniformly distributed and connected to the inner wall of the reaction cavity 1012.
Preferably, the synthesizing device further comprises two groups of bilaterally symmetrical raw material input groups, and the two groups of bilaterally symmetrical raw material input groups are respectively used for inputting liquid to the two liquid inlets 4.
The raw material input group comprises:
the storage tank 10 is fixedly connected to the left side or the right side of the upper surface of the partition board 2;
the liquid inlet funnel 11, the lower end of the liquid inlet funnel 11 is fixedly connected with a liquid inlet pipe, and the liquid inlet pipe penetrates through the shell 101 and is inserted into the storage tank 10;
and one end of the transmission pipeline 12 is communicated with the storage tank 10, the other end of the transmission pipeline 12 is connected with the inside of the corresponding liquid inlet 4, and the transmission pipeline 12 is connected with a second pressurizing pump 13.
Preferably, the mixing tank 3 is also connected with a stirring assembly.
The stirring assembly includes: a motor case 14, a motor 15, and a stirring rod 16;
the motor box 14 is fixedly connected to the outer side of the upper end of the shell 101, and the motor 15 is arranged in the motor box 14;
the upper end of the stirring rod 16 is fixedly connected with the output shaft of the motor 15, and the stirring rod 16 penetrates through the upper end of the mixing tank 3;
the lower part of the stirring rod 16 is fixedly connected with a plurality of stirring blades 17, and the stirring blades 17 are positioned in the reaction cavity 102.
Preferably, the synthesizing device further comprises a controller, and the controller is electrically connected with the first pressurizing pump 8, the second pressurizing pump 13, the motor 15 and the microwave magnetron 9.
The working principle of the technical scheme is as follows: siCl is added to 4 And NH 3 The liquid is respectively supplied into the storage tanks 10 through the liquid inlet hopper 11 for storage, when the production is started, the SiCl is pumped from the storage tanks 10 at a specified speed through the conveying pipelines 12 at the two sides 4 And NH 3 Liquid is filled into the mixing tank 3, and SiCl is stirred by the stirring assembly 4 And NH 3 The liquid is mixed uniformly, the mixed liquid is sprayed out from the sprayer 6 through the pressurizing pump I8, sprayed water mist is irradiated through the microwave magnetron 9 to react under the action of microwaves to produce alpha-phase silicon nitride powder, and after a certain amount of silicon nitride powder is generated, the blanking valve is opened to discharge the silicon nitride powder out of the synthesizing device.
The beneficial effects of the technical scheme are as follows: siCl is added to 4 And NH 3 The liquid is respectively stored, the damage to the synthesis device caused by the reaction in non-production time is prevented, and the stirring component is arranged to accelerate SiCl 4 And NH 3 The mixing of the liquid improves the efficiency of the synthesis.
The microwave heating is used, the reaction temperature is low, the safety of the synthesis process is improved, the energy loss is reduced, and the production cost is reduced.
Example 3: on the basis of embodiment 1 or 2, as shown in fig. 2-3, a sorting device 18 is further included, the sorting device 18 is disposed below the right side of the synthesizing device 1, and the sorting device 18 includes:
the device comprises a box body 181, wherein a gas tank cavity 1811 and a screening cavity 1812 are arranged in the box body 181, a chute 1813 is formed in the inner wall of the screening cavity 1812, a first opening 1814 is formed in the left side of the upper end of the box body 181, the first opening 1814 is positioned below a discharging plate 40, and the box body 181 is fixedly connected to the upper end of a bottom plate 42;
the rotating shaft 19, the rotating shaft 19 is rotationally connected with the right side of the first opening 1814, and a gear 20 is fixedly connected to the rotating shaft 19;
a protective cover 21, wherein the protective cover 21 is fixedly connected with the left end of the rotating shaft 19, the protective cover 21 is positioned above the screening cavity 1812, and the protective cover 21 is used for sealing or opening the first opening 1814;
the rack bar 22 is meshed with the gear 20 for transmission, a pressing plate 23 is fixedly connected to the top end of the rack bar 22, and a roller 24 is rotatably connected to the lower end of the rack bar 22;
two magnetic blocks 25, one magnetic block 25 is fixedly connected to the lower surface of the pressing plate 23, and the other magnetic block 25 is fixedly connected to the upper surface of the box 181;
the gas tank frame 26, the gas tank frame 26 is fixedly connected with the inner wall of the gas tank cavity 1811, and a gas storage tank 27 is arranged on the gas tank frame 26;
a collection box 28, wherein the collection box 28 is slidably connected in the chute 1813 along the up-down direction, and the side wall of the collection box 28 is provided with a vent 29;
the conical block 30 is slidably connected with the inner wall of the screening cavity 1812 along the left-right direction, the conical block 30 is positioned below the roller 24, and the roller 24 is in contact with the conical surface of the conical block 30;
a connecting rod 31, wherein one end of the connecting rod 31 is hinged with the conical block 30, and the other end of the connecting rod 31 is hinged with the bottom of the collecting box 28;
the two mounting frames 32 are fixedly connected with the inner walls of the left side and the right side of the collecting box 28 respectively, and the upper surface of the mounting frame 32 is fixedly connected with a fixing rod 33;
the cam 34 is rotationally connected with the mounting frame 32 through a rotating shaft in the front-rear direction, and a driving device is arranged on the mounting frame 32 and used for driving the cam 34 to rotate;
a vent pipe 35, one end of the vent pipe 35 is communicated with the air storage tank 27, and the other end of the vent pipe 35 penetrates through the left side wall of the air storage tank cavity 1811;
the screening barrel 36, the left portion and the right portion of screening barrel 36 all set up extension 38, and left portion and right portion extension 38 are respectively along upper and lower direction slip cup joint on corresponding dead lever 33, screening barrel 36 lower surface opening, and screening barrel 36 lower surface is provided with screen cloth 37, and the extension 38 lower extreme of left portion and right portion contacts with corresponding cam 34 respectively.
The working principle of the technical scheme is as follows: when the device is used, firstly, the pressing plate 23 is pressed down, the rack bar 22 is meshed with the gear 20, the gear 20 and the rotating shaft 19 are driven to rotate, the rotating shaft 19 rotates to drive the protective cover 21 to rotate and lift up, the rack bar 22 moves downwards to drive the roller 24 to press down so that the conical block 30 moves rightwards, the collecting box 28 is jacked up under the action of the connecting rod 31, the two magnetic blocks 25 are attracted to each other, the protective cover 21 is kept not to be covered, alpha-phase silicon nitride powder falls into the screening barrel 36 through the discharging plate 40, the pressing plate 23 is pulled, the two magnetic blocks 25 are separated, the protective cover 21 is tightly covered, the collecting box 28 falls, the cam 34 rotates under the driving of the driving device, the screening barrel 36 is jacked up periodically, the silicon nitride powder with smaller powder falls into the collecting box 28, and protective gas in the gas storage tank 27 is blown into the collecting box 28 through the ventilation pipeline 35 to accelerate the drying of the silicon nitride powder and protect the silicon nitride powder from deterioration.
The beneficial effects of the technical scheme are as follows: under the condition that the pressing plate 23 is not used, the air vent 29 is staggered with the air duct 35 after the collecting box 28 is jacked up, the air storage tank 27 stops blowing air into the collecting box 28, the protection gas is saved, the waste of the gas is prevented, the protection gas is adopted to blow, the silicon nitride powder is prevented from deteriorating, the quality of the silicon nitride powder is improved, the thinner silicon nitride powder is separated from the thicker silicon nitride powder, the silicon nitride powder with different quality can be used in different requirements, the maximum value of the silicon nitride powder with different quality can be exerted, the collecting box 28 is jacked up when the protective cover 21 is opened, the silicon nitride powder in the collecting box 28 is conveniently collected by operators, the screening barrel 36 is slidably connected on the fixing rod 33, the silicon nitride powder in the screening barrel 36 and in the collecting box 28 can be conveniently taken down, and the cam 34 is arranged to periodically jack up the screening barrel 36, and the screening effect can be effectively improved.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (8)
1. The synthesis method of the high alpha-phase silicon nitride powder is characterized by comprising the following steps of:
step one: siCl is added to 4 NH (NH) 3 Mixing the liquid;
step two: the SiCl obtained in the step one is treated 4 NH (NH) 3 Spraying the liquid mixture into a reaction cavity with a microwave magnetron through a nozzle, and SiCl 4 NH (NH) 3 The liquid mixture reacts by microwave action to produce alpha phase silicon nitride powder.
2. A method of synthesizing high alpha phase silicon nitride powder according to claim 1, wherein the first and second steps are performed based on a production apparatus including a synthesizing apparatus (1), the synthesizing apparatus (1) including:
the device comprises a shell (101), wherein a partition plate (2) is fixedly connected inside the shell (101), the partition plate (2) divides the inside of the shell (101) into a mixing cavity (1011) and a reaction cavity (1012), the reaction cavity (1012) is positioned below the mixing cavity (1011), the lower end of the shell (101) is connected with a fixing bracket (41), and the fixing bracket (41) is fixedly connected with the upper end of a bottom plate (42);
the mixing tank (3), the mixing tank (3) is fixedly connected with the upper surface of the partition board (2), two liquid inlets (4) are symmetrically formed in the left and right of the upper end of the mixing tank (3), and a liquid outlet (5) is formed in the lower end of the mixing tank (3);
the sprayer (6) is fixedly connected to the lower surface of the partition board (2);
one end of the infusion tube (7) is communicated with the liquid outlet (5), the other end of the infusion tube (7) is communicated with the liquid inlet of the sprayer (6), and the infusion tube (7) is connected with a first booster pump (8);
the discharging plate (40), the discharging plate (40) is fixedly connected to the lower side of the right wall of the reaction cavity (1012), and the discharging plate (40) is connected with a blanking valve (39);
and the plurality of microwave magnetrons (9) are uniformly distributed and connected to the inner wall of the reaction cavity (1012).
3. A method of synthesizing a high alpha phase silicon nitride powder as claimed in claim 2, wherein said synthesizing apparatus further comprises two sets of bilaterally symmetrical raw material input sets for inputting liquid to the two liquid inlets (4), respectively.
4. A method of synthesizing high alpha phase silicon nitride powder as defined in claim 3 wherein said feedstock input set comprises:
the storage tank (10) is fixedly connected to the left side or the right side of the upper surface of the partition board (2);
the liquid inlet funnel (11), the lower end of the liquid inlet funnel (11) is fixedly connected with a liquid inlet pipe, and the liquid inlet pipe penetrates through the shell (101) and is inserted into the storage tank (10);
the device comprises a transmission pipeline (12), wherein one end of the transmission pipeline (12) is communicated with a storage tank (10), the other end of the transmission pipeline (12) is connected with a corresponding liquid inlet (4), and a second pressurizing pump (13) is connected to the transmission pipeline (12).
5. A method of synthesizing a high alpha phase silicon nitride powder as claimed in claim 4 wherein said mixing tank (3) is further connected with a stirring assembly.
6. A method of synthesizing high alpha phase silicon nitride powder according to claim 5, wherein the stirring assembly comprises: a motor case (14), a motor (15) and a stirring rod (16);
the motor box (14) is fixedly connected to the outer side of the upper end of the shell (101), and the motor (15) is arranged in the motor box (14);
the upper end of the stirring rod (16) is fixedly connected with an output shaft of the motor (15), and the stirring rod (16) penetrates through the upper end of the mixing tank (3);
the lower part of the stirring rod (16) is fixedly connected with a plurality of stirring blades (17), and the stirring blades (17) are positioned in the reaction cavity (102).
7. A method of synthesizing high alpha phase silicon nitride powder as defined in claim 6 wherein said synthesizing apparatus further comprises a controller electrically connected to said first booster pump (8), said second booster pump (13), said motor (15) and said microwave magnetron (9).
8. A method of synthesizing high alpha phase silicon nitride powder as claimed in claim 2 further comprising a sorting device (18), said sorting device (18) being disposed below the right side of the synthesizing device (1), said sorting device (18) comprising:
the device comprises a box body (181), wherein a gas tank cavity (1811) and a screening cavity (1812) are formed in the box body (181), a chute (1813) is formed in the inner wall of the screening cavity (1812), a first opening (1814) is formed in the left side of the upper end of the box body (181), the first opening (1814) is located below a discharging plate (40), and the box body (181) is fixedly connected to the upper end of a bottom plate (42);
the rotating shaft (19), the rotating shaft (19) is rotationally connected with the right side of the first opening (1814), and a gear (20) is fixedly connected to the rotating shaft (19);
the protective cover (21), the said protective cover (21) is fixedly connected with left end of the rotary shaft (19), the said protective cover (21) locates above screening cavity (1812), the protective cover (21) is used for sealing or opening the first opening (1814);
the rack bar (22) is meshed with the gear (20) for transmission, a pressing plate (23) is fixedly connected to the top end of the rack bar (22), and a roller (24) is rotatably connected to the lower end of the rack bar (22);
two magnetic blocks (25), one magnetic block (25) is fixedly connected to the lower surface of the pressing plate (23), and the other magnetic block (25) is fixedly connected to the upper surface of the box body (181);
the gas tank comprises a gas tank frame (26), wherein the gas tank frame (26) is fixedly connected with the inner wall of a gas tank cavity (1811), and a gas storage tank (27) is arranged on the gas tank frame (26);
the collecting box (28) is connected in the chute (1813) in a sliding manner along the up-down direction, and a vent hole (29) is formed in the side wall of the collecting box (28);
the conical block (30) is slidably connected with the inner wall of the screening cavity (1812) along the left-right direction, the conical block (30) is positioned below the roller (24), and the roller (24) is in contact with the conical surface of the conical block (30);
the connecting rod (31), one end of the connecting rod (31) is hinged with the conical block (30), and the other end of the connecting rod (31) is hinged with the bottom of the collecting box (28);
the two mounting frames (32), the two mounting frames (32) are fixedly connected with the inner walls of the left side and the right side of the collecting box (28) respectively, and the upper surface of each mounting frame (32) is fixedly connected with a fixing rod (33);
the cam (34) is rotationally connected with the mounting frame (32) through a rotating shaft in the front-rear direction, and a driving device is arranged on the mounting frame (32) and used for driving the cam (34) to rotate;
one end of the ventilation pipeline (35) is communicated with the air storage tank (27), and the other end of the ventilation pipeline (35) penetrates through the left side wall of the air storage tank cavity (1811);
screening bucket (36), the left portion and the right part of screening bucket (36) all set up extension (38), and left portion and right part extension (38) are respectively along upper and lower direction slip cup joint on corresponding dead lever (33), screening bucket (36) lower surface opening, and screening bucket (36) lower surface is provided with screen cloth (37), and extension (38) lower extreme of left portion and right part respectively with corresponding cam (34) contact.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116693301A (en) * | 2023-06-01 | 2023-09-05 | 衡阳凯新特种材料科技有限公司 | Method for preparing silicon nitride powder by continuous ammonolysis method |
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