CN116693301A - Method for preparing silicon nitride powder by continuous ammonolysis method - Google Patents
Method for preparing silicon nitride powder by continuous ammonolysis method Download PDFInfo
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- CN116693301A CN116693301A CN202310642660.9A CN202310642660A CN116693301A CN 116693301 A CN116693301 A CN 116693301A CN 202310642660 A CN202310642660 A CN 202310642660A CN 116693301 A CN116693301 A CN 116693301A
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 93
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 239000000843 powder Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 44
- 238000005915 ammonolysis reaction Methods 0.000 title claims abstract description 25
- 239000002243 precursor Substances 0.000 claims abstract description 42
- 230000007246 mechanism Effects 0.000 claims abstract description 30
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 238000002360 preparation method Methods 0.000 claims abstract description 17
- 238000012545 processing Methods 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 11
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000005049 silicon tetrachloride Substances 0.000 claims abstract description 9
- 238000010304 firing Methods 0.000 claims description 16
- 238000006073 displacement reaction Methods 0.000 claims description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 9
- 238000007790 scraping Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical group ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000007796 conventional method Methods 0.000 abstract 1
- 238000005192 partition Methods 0.000 description 10
- 230000002457 bidirectional effect Effects 0.000 description 9
- 239000007789 gas Substances 0.000 description 7
- 239000012295 chemical reaction liquid Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000002309 gasification Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000003915 air pollution Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
- B01J6/001—Calcining
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B17/00—Furnaces of a kind not covered by any preceding group
- F27B17/0016—Chamber type furnaces
- F27B17/0041—Chamber type furnaces specially adapted for burning bricks or pottery
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
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- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention provides a method for preparing silicon nitride powder by a continuous ammonolysis method, which relates to the technical field of silicon nitride preparation and comprises the following steps: adding a solvent and silicon tetrachloride required for preparing silicon nitride powder into a reaction container of an integrated preparation device; introducing liquid ammonia into a reaction container of the integrated preparation device, and reacting with the solution obtained in the step one to obtain a silicon nitride precursor; and conveying the silicon nitride precursor to a processing mechanism of the integrated preparation device for processing, so as to obtain silicon nitride powder. By designing a method for preparing silicon nitride powder by a continuous ammonolysis method, the problem that the production efficiency of silicon nitride is low due to the fact that a silicon nitride precursor is manually taken out after the reaction is finished and then is subjected to subsequent operation in the conventional method for preparing silicon nitride powder by the ammonolysis method is effectively solved.
Description
Technical Field
The invention relates to the technical field of silicon nitride preparation, in particular to a method for preparing silicon nitride powder by a continuous ammonolysis method.
Background
Silicon nitride is an inorganic substance, is an important structural ceramic material, has high hardness, has lubricating property, is wear-resistant, and is an atomic crystal; oxidation resistance at high temperature. It can resist cold and hot impact, and can be heated to above 1000 deg.C in air, and can be quickly cooled and then quickly heated, and can not be broken. Because of the excellent properties of silicon nitride ceramics, it is often used to manufacture mechanical components such as bearings, turbine blades, mechanical seal rings, permanent molds, and the like. If the heating surface of the engine part is made of the silicon nitride ceramics with high resistance Wen Erju and difficult heat transfer, the quality of the diesel engine can be improved, the fuel can be saved, and the heat efficiency can be improved.
The existing method for preparing silicon nitride powder by an ammonolysis method generally comprises the steps of manually taking out a silicon nitride precursor (one existing form before a target product is obtained) after the reaction is finished, and then carrying out subsequent operation on the silicon nitride precursor, so that the problem of low production efficiency of silicon nitride is solved. Therefore, in view of the above-mentioned current situation, there is an urgent need to develop a method for preparing silicon nitride powder by continuous ammonolysis, so as to overcome the defects in the current practical application.
Disclosure of Invention
The invention provides a method for preparing silicon nitride powder by a continuous ammonolysis method, which is used for solving the problems set forth in the background art: the existing method for preparing silicon nitride powder by an ammonolysis method generally takes out the silicon nitride precursor manually after the reaction is finished, and then carries out subsequent operation on the silicon nitride precursor, so that the problem of low production efficiency of silicon nitride is solved.
In order to solve the technical problems, the invention discloses a method for preparing silicon nitride powder by a continuous ammonolysis method, which comprises the following steps:
step one: adding a solvent and silicon tetrachloride required for preparing silicon nitride powder into a reaction container of an integrated preparation device;
step two: introducing liquid ammonia into a reaction container of the integrated preparation device, and reacting with the solution obtained in the step one to obtain a silicon nitride precursor;
step three: and conveying the silicon nitride precursor to a processing mechanism of the integrated preparation device for processing, so as to obtain silicon nitride powder.
Preferably, the solvent added in step one is ethylene dichloride and hexane.
Preferably, the internal temperature of the reaction vessel is controlled between-25 ℃ and-35 ℃.
Preferably, the liquid ammonia in the second step is introduced at a speed of 1-5L/min, and the liquid ammonia gasification speed is 0.8-4.5L/min.
Preferably, the reaction vessel comprises: the device comprises a first box body, a first connecting pipe and a second connecting pipe are fixedly installed on the top end of the first box body from left to right, one end of the third connecting pipe is connected with the input end of the pressurizing and air dissolving device, the other end of the third connecting pipe is communicated with the first box body, the output end of the pressurizing and air dissolving device is communicated with the first box body, a partition plate is fixedly installed on the inner wall of the first box body, the middle end of the partition plate is fixedly connected with the fourth connecting pipe, a first valve is fixedly installed on the fourth connecting pipe, a second valve is arranged on the right side of the bottom end of the first box body, a filter plate is fixedly installed on the inner wall of the bottom end of the first box body, a cavity at the bottom end of the filter plate is communicated with the fifth end of the connecting pipe, the other end of the fifth connecting pipe is communicated with the cavity at the top end of the partition plate, a water pump is fixedly installed on the fifth connecting pipe, and a scraping mechanism is arranged at the bottom end at the left side of the first box body.
Preferably, the scraping mechanism includes: the first driving motor is fixedly arranged on the inner wall of the bottom end at the left side of the first box body, the first driving motor is fixedly arranged on the inner wall of the second box body, the first driving motor is fixedly provided with a first gear, the first gear is meshed with the second gear, the second gear is fixedly arranged on a first rotating shaft, the front end and the rear end of the first rotating shaft are rotatably connected on the inner wall of the second box body, swinging rods are fixedly arranged on the rotating shafts at the front end and the rear end of the second gear respectively, the eccentric center of the swinging rods are fixedly connected with the first rotating shaft, the right side of the swinging rods are in contact with a displacement rod, the displacement rod penetrates through the second box body and is fixedly connected with a push rod, the left end of a reset spring is fixed on the displacement rod, and the right end of the reset spring is fixed on the inner wall of the second box body.
Preferably, the processing mechanism includes: the treatment box is fixedly connected with the first box body, the bottom end of a cavity body arranged at the left side of the treatment box is communicated with the first box body, the top end of the cavity body is communicated with the burning chamber, the first cavity body is rotationally connected with a packing auger, the top end of the packing auger penetrates through the first cavity body and is fixedly connected with the first bevel gear, the first bevel gear is meshed with the second bevel gear, one end of the second rotating shaft is fixedly connected with the second bevel gear, the other end of the second rotating shaft is fixedly connected with the third bevel gear, the third bevel gear is connected with the driving mechanism, the belt pulley I is fixedly arranged on the rotating shaft II, the belt pulley II is fixedly arranged on the rotating shaft III, the belt pulley I is connected with the belt pulley II through a first belt, one end of the rotating shaft III is rotationally connected in a cavity II where the belt pulley II is arranged, the other end of the rotating shaft III is rotationally connected on the inner wall of the burning chamber, a plurality of stirring blades are fixedly arranged on the rotating shaft III, a burning device is fixedly arranged on the inner wall of the top end of the burning chamber, and a valve III is arranged at the bottom end of the burning chamber.
Preferably, the driving mechanism includes: the motor is fixedly arranged in a cavity III arranged in the treatment box, an output shaft of the motor is fixedly provided with a gear III, the gear III is meshed with a rack, a sliding block is fixedly arranged on the left side of the rack, the sliding block is vertically and slidably connected in a sliding groove formed in the cavity III, a bidirectional driving motor is fixedly arranged on the rack, an output shaft at the top end of the bidirectional driving motor is in non-fixed spline connection with one end of a rotating shaft, a bevel gear IV is fixedly arranged at the other end of the rotating shaft, the bevel gear IV is meshed with the bevel gear III, an output shaft at the bottom end of the bidirectional driving motor is in non-fixed spline connection with one end of a worm, the other end of the worm is rotationally connected to the inner wall at the bottom end of the cavity IV, and the bevel gear V is fixedly arranged on the worm.
Preferably, still be equipped with broken mechanism in the processing case, broken mechanism includes: the worm wheel is meshed with a worm arranged in the driving mechanism, a belt pulley III is fixedly arranged on the worm wheel, the driving roller and the driven roller are respectively and rotatably connected to the inner wall of the crushing chamber, the rear ends of the driving roller and the driven roller are connected through a second belt, the front end of the driving roller is fixedly provided with a belt pulley IV, the belt pulley III is connected with the belt pulley IV through a third belt, the five end of a rotating shaft is fixedly connected with a bevel gear V, the five other end of the rotating shaft penetrates through the crushing chamber and is rotatably connected with the inner wall of the crushing chamber, a plurality of crushing rods are fixedly arranged on the five rotating shaft, the bevel gear V is meshed with the bevel gear V, and a plurality of crushing balls are arranged in the crushing chamber.
Preferably, a roasting chamber is further arranged in the treatment box, the roasting chamber is arranged at the bottom end of the crushing chamber, six ends of the connecting pipe are communicated with the crushing chamber, the six other ends of the connecting pipe are connected with the input end of the powder suction device, and the output end of the powder suction device is communicated with the roasting chamber.
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 schematic diagram of a process for preparing silicon nitride powder according to the present invention;
FIG. 2 is a schematic view of an internal structure of the case of the present invention;
FIG. 3 is a top view of a second embodiment of the case of the present invention;
FIG. 4 is an enlarged partial schematic view of FIG. 2 in accordance with the present invention;
fig. 5 is an enlarged schematic view of the point a in fig. 4 according to the present invention.
In the figure: 1. a first box body; 2. a first connecting pipe; 3. a second connecting pipe; 4. a third connecting pipe; 5. a pressurized air dissolving device; 6. a partition plate; 7. a connecting pipe IV; 8. a valve I; 9. a second valve; 10. a filter plate; 11. a fifth connecting pipe; 12. a water pump; 13. a second box body; 14. driving a first motor; 15. a first gear; 16. a second gear; 17. a first rotating shaft; 18. a swinging rod; 19. a displacement rod; 20. a push rod; 21. a return spring; 22. a treatment box; 23. a first cavity; 24. an auger; 25. bevel gears I; 26. bevel gears II; 27. a second rotating shaft; 28. bevel gears III; 29. a first belt pulley; 30. a third rotating shaft; 31. stirring blades; 32. a burning device; 33. a third valve; 34. a second cavity; 35. a belt pulley II; 36. a motor; 37. a cavity III; 38. a third gear; 39. a rack; 40. a slide block; 41. a bi-directional drive motor; 42. a rotation shaft IV; 43. bevel gears IV; 44. a worm; 45. a cavity IV; 46. a bevel gear V; 47. a worm wheel; 48. a belt pulley III; 49. a drive roll; 50. a crushing chamber; 51. a belt pulley IV; 52. a fifth rotating shaft; 53. a bevel gear six; 54. a breaker bar; 55. crushing balls; 56. driven roller; 57. a roasting chamber; 58. a connecting pipe six; 59. a powder suction device; 60. a firing chamber.
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, the descriptions of the "first," "second," and the like, herein are for descriptive purposes only and are not intended to be specifically construed as order or sequence, nor are they intended to limit the invention solely for distinguishing between components or operations described in the same technical term, but are not to be construed as indicating or implying any relative importance or order of such features. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. 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.
The invention provides the following examples
Example 1
The embodiment of the invention provides a method for preparing silicon nitride powder by a continuous ammonolysis method, which is shown in figure 1 and comprises the following steps:
step one: adding a solvent and silicon tetrachloride required for preparing silicon nitride powder into a reaction container of an integrated preparation device;
step two: introducing liquid ammonia into a reaction container of the integrated preparation device, and reacting with the solution obtained in the step one to obtain a silicon nitride precursor;
step three: and conveying the silicon nitride precursor to a processing mechanism of the integrated preparation device for processing, so as to obtain silicon nitride powder.
Optionally, the solvent added in the first step is ethylene dichloride and hexane.
Optionally, the internal temperature of the reaction vessel is controlled between-25 ℃ and-35 ℃.
Optionally, the liquid ammonia in the second step is introduced at a speed of 1-5L/min, and the liquid ammonia gasification speed is 0.8-4.5L/min.
The beneficial effects of the technical scheme are as follows: according to the method for preparing the silicon nitride powder by the continuous ammonolysis method, the integrated preparation device is arranged, the solvent, the silicon tetrachloride and the liquid ammonia required for preparing the silicon nitride powder are continuously added into the reaction container of the integrated preparation device to obtain the silicon nitride precursor, and the silicon nitride precursor is automatically sent into the treatment mechanism of the integrated preparation device for treatment, so that the silicon nitride powder is obtained, the silicon nitride powder is continuously generated, the continuity of the working procedure is realized, and manual operation is not needed, so that the existing method for preparing the silicon nitride powder by the ammonolysis method is effectively solved, the silicon nitride precursor is manually taken out after the reaction is finished, and then the subsequent treatment is carried out, so that the production efficiency of the silicon nitride is reduced; according to the invention, the internal temperature of the reaction vessel is controlled, so that the solvent, silicon tetrachloride and liquid ammonia required for preparing the silicon nitride powder are always kept in a liquid state, and the reaction speed is improved; through the speed of letting in of control liquid ammonia and liquid ammonia gasification speed, be favorable to making liquid ammonia and silicon tetrachloride can fully contact, improve the speed of reaction, can control the particle size of silicon nitride precursor through the speed of liquid ammonia letting in and gasification speed moreover.
Example 2
Based on the embodiment 1, as shown in fig. 2-3, a method for preparing silicon nitride powder by a continuous ammonolysis method, a reaction vessel comprises: the device comprises a first box body 1, wherein a first connecting pipe 2 and a second connecting pipe 3 are fixedly arranged at the top end of the first box body 1 from left to right, one end of a third connecting pipe 4 is connected with the input end of a pressurizing and air dissolving device 5 (refer to an intelligent pressurizing and air dissolving device disclosed by CN 208776350U), the other end of the third connecting pipe 4 is communicated with the first box body 1, the output end of the pressurizing and air dissolving device 5 is communicated with the first box body 1, a baffle 6 is fixedly arranged on the inner wall of the first box body 1, the middle end of the baffle 6 is fixedly connected with a fourth connecting pipe 7, a first valve 8 is fixedly arranged on the fourth connecting pipe 7, a second valve 9 is arranged on the right side of the bottom end of the first box body 1, a filter plate 10 is fixedly arranged on the inner wall of the bottom end of the first box body 1, a cavity at the bottom end of the filter plate 10 is communicated with one end of a fifth connecting pipe 11, the other end of the fifth connecting pipe 11 is communicated with the cavity where the top end of the baffle 6 is located, a water pump 12 is fixedly arranged on the fifth connecting pipe 11, and a scraping mechanism is arranged at the left side bottom end of the first box body 1.
Optionally, the scraping mechanism includes: the box body II 13, box body II 13 fixed mounting is on the left side bottom inner wall of box body I1, driving motor I14 fixed mounting is on the box body II 13 inner wall, and driving motor I14's output shaft fixed mounting has gear I15, gear I15 and gear II 16 meshing, gear II 16 fixed mounting is on pivot I17, both ends rotate around the pivot I17 and connect on the box body II 13 inner wall, and respectively fixed mounting has swinging arms 18 on pivot I17 at both ends around the gear II 16, swinging arms 18 eccentric center department and pivot I17 fixed connection, and the right side of swinging arms 18 contacts with displacement rod 19, displacement rod 19 runs through box body II 13 and push rod 20 fixed connection, the left end of return spring 21 is fixed on displacement rod 19, the right-hand member of return spring 21 is fixed on the box body II 13 inner wall.
The working principle of the technical scheme is as follows: the method comprises the steps of introducing solvent and silicon tetrachloride solution required for preparing silicon nitride powder from a first connecting pipe 2, introducing liquid ammonia from a second connecting pipe 3 (at the moment, a first valve 8 is in an open state), regulating the temperature in a first box body 1 to minus 25 to minus 35 ℃ to enable the liquid ammonia to fully react, generating liquid ammonia under the action of a pressurizing and gas dissolving device 5 from a third connecting pipe 4 after gasifying the liquid ammonia, introducing the liquid ammonia into the first box body 1 again to react, closing the first valve 8 after reacting for a certain time, then starting a water pump 12, conveying reaction liquid at the bottom end of a partition plate 6 filtered by the water pump 12 from a fifth connecting pipe 11 into the first box body 1 at the top end of the partition plate 6, attaching a silicon nitride precursor generated by the reaction to the inner wall at the bottom end of the first box body 1, starting a driving motor 14, opening the second valve 9, driving the first gear 15 to rotate by the driving motor 14, driving a gear 16 meshed with the first gear 15 to rotate, driving a rotating shaft 17 to rotate by the rotation of the gear 16, swinging a swinging rod 18 fixedly arranged with the rotating shaft 17, driving the swinging rod 18 to swing, driving the swinging rod 18 to move the partition plate 6 to move to the top end of the partition plate 6, and pushing the silicon nitride precursor to the inner wall 20 to the right, and pushing the silicon nitride precursor to the inner wall to the first box body to move to the right.
The beneficial effects of the technical scheme are as follows: the first connecting pipe 2 and the second connecting pipe 3 are arranged, so that solvent, silicon tetrachloride solution and liquid ammonia required for preparing silicon nitride powder can be continuously introduced into the first box 1, the device can always keep a continuous reaction state, vaporized ammonia can be conveniently formed again through the pressurization by the aid of the pressurizing gas dissolving device 5, reaction requirements are met, cost of the liquid ammonia is further reduced, and meanwhile, the ammonia is prevented from being directly discharged into air to cause air pollution; the first valve 8 is closed, and the filter plate 10 is arranged, so that the silicon nitride precursor and the reaction liquid are separated, and the silicon nitride precursor is treated; the water pump 12 is arranged, so that the reaction liquid in the first box body 1 at the bottom end of the partition plate 6 is conveyed into the first box body 1 at the top end of the partition plate 6; through setting up and scraping the mechanism, be favorable to scraping the silicon nitride precursor that 1 bottom inner wall reaction of box generated to in the pushing treatment mechanism, very convenient and practical.
Example 3
On the basis of embodiment 1 or 2, as shown in fig. 4 to 5, the processing mechanism includes: the treatment box 22, the treatment box 22 and the first 1 fixed connection of box, and the cavity one 23 bottom that the treatment box 22 left side was established communicates with first 1 of box, cavity one 23 top and firing chamber 60 intercommunication (firing temperature control in the firing chamber 60 is 120 ℃, time is 30min, can let in the protection gas in the firing chamber, protection gas is one of nitrogen gas, helium or argon gas), and cavity one 23 internal rotation is connected with auger 24, auger 24 top runs through cavity one 23 and bevel gear one 25 fixed connection, bevel gear one 25 and bevel gear two 26 meshing connection, bevel gear two 27 one end and bevel gear two 26 fixed connection, the other end and bevel gear three 28 fixed connection of pivot two 27, bevel gear three 28 is connected with actuating mechanism, belt pulley one 29 fixed mounting is on pivot two 27, belt pulley two 35 fixed mounting is on pivot three 30, and belt pulley one 29 is connected through first belt pulley three 30 one end rotation is connected in the cavity two 34 of belt pulley two 35, the pivot three 30 other end rotation is connected on the inner wall of chamber 60, and three 30 fixed mounting has blade 31 to be equipped with firing instrument three firing devices on the inner wall of pivot three 30, and three firing instrument 35 fixed mounting on the inner wall of the chamber 60 CN is equipped with three bottom end of reference chamber 60 (32).
Optionally, the driving mechanism includes: the motor 36, motor 36 fixed mounting is in the cavity third 37 that processing box 22 set up, and the output shaft fixed mounting of motor 36 has gear third 38, gear third 38 and rack 39 meshing, rack 39 left side fixed mounting has slider 40, slider 40 sliding connection is in the spout that cavity third 37 was established from top to bottom, and fixed mounting has two-way driving motor 41 on rack 39, two-way driving motor 41 top output shaft and the unsteady spline connection of pivot fourth 42 one end, pivot fourth 42 other end fixed mounting has bevel gear fourth 43, bevel gear fourth 43 and bevel gear third 28 meshing, two-way driving motor 41 bottom output shaft and the unsteady spline connection of worm 44 one end, the worm 44 other end swivelling joint is on the bottom inner wall of cavity fourth 45, and fixed mounting has bevel gear fifth 46 on the worm 44.
The working principle of the technical scheme is as follows: when the silicon nitride precursor needs to be burnt, the motor 36 is started firstly, the motor 36 rotates to drive the gear III 38 to rotate clockwise, so that the rack 39 is driven to slide upwards until an output shaft at the top end of the bidirectional driving motor 41 is in spline connection with the rotating shaft IV 42, then the bidirectional driving motor 41 is started, the bidirectional driving motor 41 rotates to drive the rotating shaft IV 42 and the bevel gear IV 43 fixedly connected with the rotating shaft IV 42 to rotate, the bevel gear IV 43 rotates to drive the bevel gear III 28 meshed with the rotating shaft IV to rotate, the bevel gear II 26 fixedly arranged on the rotating shaft II 27 is further driven to rotate with the belt pulley I29, the bevel gear II 26 rotates to drive the bevel gear I25 meshed with the bevel gear II to rotate, the valve II 9 is opened simultaneously, the silicon nitride precursor is conveyed into the burning chamber 60 through the auger 24, then the burning device 32 is started, the silicon nitride precursor in the burning chamber 60 is burnt, the belt pulley I29 rotates to drive the belt pulley II 35 connected with the second belt of the silicon nitride precursor, and the rotating shaft III and the stirring blade 31 are driven to rotate, so that the silicon nitride precursor in the burning chamber 60 is stirred sufficiently, and the silicon nitride precursor in the burning chamber 60 is burnt.
The beneficial effects of the technical scheme are as follows: the burning chamber 60 is arranged, so that the reaction liquid existing in the silicon nitride precursor body is cleaned, and the purity of the reaction liquid is improved; by arranging the valve II 9, the reaction solution is prevented from entering the cavity I23 through the valve II 9 in the reaction process; by providing the auger 24, the low-point silicon nitride precursor is advantageously conveyed into the firing chamber 60 through the auger 24; by arranging the burning device 32, the burning treatment of the silicon nitride precursor is facilitated; the rotating shaft III 30 and the stirring blade 31 are arranged, so that the silicon nitride precursor in the firing chamber 60 is raised, the silicon nitride precursor in the firing chamber 60 is fully fired, insufficient firing of the silicon nitride precursor at the bottom end of the firing chamber 60 is prevented, and the next treatment is influenced; through setting up motor 36 and two-way driving motor 41, be favorable to realizing that a small amount of drives and drives the overall operation to reduce the use of electric energy, further reduce the vibrations that the motor rotation produced and to the influence of spare part, very convenient and practical.
Example 4
In addition to embodiment 3, as shown in fig. 4, a crushing mechanism is further provided in the processing box 22, and the crushing mechanism includes: the worm wheel 47, worm wheel 47 meshes with worm 44 that sets up in the actuating mechanism, and fixedly mounted with belt pulley three 48 on the worm wheel 47, drive roll 49 and driven voller 56 rotate respectively and connect on crushing room 50 inner wall, and drive roll 49 passes through the second belt with driven voller 56 rear end and is connected, drive roll 49 front end fixed mounting has belt pulley four 51, belt pulley three 48 passes through the third belt with belt pulley four 51 and is connected, pivot five 52 one end and bevel gear six 53 fixed connection, the pivot five 52 other end runs through crushing room 50, and rotate with crushing room 50 inner wall and be connected, and fixedly mounted with a plurality of crushing poles 54 on pivot five 52, bevel gear six 53 meshes with bevel gear five 46, a plurality of crushing balls 55 set up in crushing room 50.
Optionally, a roasting chamber 57 (the roasting temperature of the roasting chamber 57 is controlled to 900 ℃ for 60min, and protective gas can be introduced into the roasting chamber 57, wherein the protective gas is one of nitrogen, helium or argon), the roasting chamber 57 is arranged at the bottom end of the crushing chamber 50, one end of a connecting pipe six 58 is communicated with the crushing chamber 50, the other end of the connecting pipe six 58 is connected with an input end of a powder suction device 59 (the powder suction device 59 can refer to CN 213859938U, a vacuum powder suction machine for mortar production, and the connecting pipe six 58 can refer to a first vertical pipeline), and an output end of the powder suction device 59 is communicated with the roasting chamber 57).
The working principle of the technical scheme is as follows: when the silicon nitride precursor is required to be crushed, the motor 36 is started firstly, the motor 36 rotates to drive the gear III 38 to rotate anticlockwise, so as to drive the rack 39 to slide downwards, until an output shaft at the bottom end of the bidirectional drive motor 41 is in spline connection with the worm 44, then the bidirectional drive motor 41 is started, the bidirectional drive motor 41 rotates to drive the worm 44 to rotate, the worm 44 rotates to drive the worm wheel 47 meshed with the worm 44 to rotate, the worm wheel 47 rotates to drive the pulley IV 51 fixed with the worm wheel, the pulley IV 51 rotates to drive the drive roller 49 and the driven roller 56 connected with the drive roller 49 to rotate, the worm 44 rotates to drive the bevel gear V46 fixedly connected with the worm wheel IV, further drive the bevel gear VI 53 meshed with the bevel gear V46 to rotate, so as to drive the crushing rods 54 fixed with the rotating shaft V46 to rotate, then the valve III 33 is opened, the burnt silicon nitride precursor is introduced into the crushing chamber 50, the silicon nitride precursor is crushed under the action of the crushing rods 54 and the driven roller 55, finally, after the crushing is completed, the powder absorbing device 59 is started, the crushed powder in the crushing chamber 50 is conveyed into the baking powder 57 through the connecting pipe 58, and the baking powder is obtained.
The beneficial effects of the technical scheme are as follows: by arranging the crushing mechanism, the burnt silicon nitride precursor is fully crushed; by arranging the driving roller 49 and the driven roller 56, the preliminary crushing treatment of the silicon nitride precursor is facilitated; by arranging the crushing rod 54 and the crushing ball 55, the crushing ball 55 is driven to roll up and down in the crushing chamber 50 through the crushing treatment of the crushing rod 54, so that the crushing effect of the silicon nitride precursor in the crushing chamber 50 is further improved, and the granularity of the silicon nitride precursor is lower; by arranging the powder suction device 59, the silicon nitride powder in the crushing chamber 50 is conveyed into the roasting chamber 57 to be subjected to final treatment, so that the purity of the silicon nitride is improved, and the method is very convenient and practical.
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 (10)
1. A method for preparing silicon nitride powder by a continuous ammonolysis method, which is characterized by comprising the following steps:
step one: adding a solvent and silicon tetrachloride required for preparing silicon nitride powder into a reaction container of an integrated preparation device;
step two: introducing liquid ammonia into a reaction container of the integrated preparation device, and reacting with the solution obtained in the step one to obtain a silicon nitride precursor;
step three: and conveying the silicon nitride precursor to a processing mechanism of the integrated preparation device for processing, so as to obtain silicon nitride powder.
2. A method for preparing silicon nitride powder by continuous ammonolysis as recited in claim 1, wherein the solvent added in step one is ethylene dichloride and hexane.
3. A method for preparing silicon nitride powder by continuous ammonolysis method according to claim 1, wherein the internal temperature of the reaction vessel is controlled between-25 ℃ and-35 ℃.
4. The method for preparing silicon nitride powder by a continuous ammonolysis method according to claim 1, wherein the liquid ammonia flowing speed in the second step is 1-5L/min, and the liquid ammonia gasifying speed is 0.8-4.5L/min.
5. A method for preparing silicon nitride powder by continuous ammonolysis as recited in claim 1, wherein the reaction vessel comprises: the novel filter comprises a first box body (1), a first connecting pipe (2) and a second connecting pipe (3) are fixedly installed at the top end of the first box body (1) from left to right, one end of the third connecting pipe (4) is connected with the input end of a pressurizing and air dissolving device (5), the other end of the third connecting pipe is communicated with the first box body (1), the output end of the pressurizing and air dissolving device (5) is communicated with the first box body (1), a baffle plate (6) is fixedly installed on the inner wall of the first box body (1), the middle end of the baffle plate (6) is fixedly connected with a fourth connecting pipe (7), a first valve (8) is fixedly installed on the fourth connecting pipe (7), a second valve (9) is arranged on the right side of the bottom end of the first box body (1), a filter plate (10) is fixedly installed on the inner wall of the bottom end of the first box body (1), the bottom end of the filter plate (10) is communicated with one end of the fifth connecting pipe (11), the other end of the fifth connecting pipe (11) is communicated with the top end of the baffle plate (6), a water pump (12) is fixedly installed on the fifth connecting pipe (11), and a scraping mechanism is arranged at the left bottom end of the first box body (1).
6. A method for preparing silicon nitride powder by continuous ammonolysis as recited in claim 5, wherein the scraping mechanism comprises: the box body II (13), box body II (13) fixed mounting is on box body I (1) left side bottom inner wall, driving motor I (14) fixed mounting is on box body II (13) inner wall, and driving motor I's (14) output shaft fixed mounting has gear I (15), gear I (15) and gear II (16) meshing, gear II (16) fixed mounting is on pivot I (17), both ends are rotated around pivot I (17) and are connected on box body II (13) inner wall, and respectively fixed mounting has swinging rod (18) on both ends pivot I (17) around gear II (16), swinging rod (18) off-axis department and pivot I (17) fixed connection, and swinging rod (18) right side and displacement rod (19) contact, displacement rod (19) run through box body II (13) and push rod (20) fixed connection, reset spring (21) left end is fixed on displacement rod (19), reset spring (21) right-hand member is fixed on box body II (13) inner wall.
7. A method for preparing silicon nitride powder by continuous ammonolysis as recited in claim 5, wherein said processing means comprises: the treatment box (22), the treatment box (22) is fixedly connected with first box (1), and cavity one (23) bottom and first box (1) intercommunication of cavity one (23) bottom that establishes in the left side of treatment box (22), cavity one (23) top and firing chamber (60) intercommunication, and cavity one (23) internal rotation is connected with auger (24), auger (24) top runs through cavity one (23) and bevel gear one (25) fixed connection, bevel gear one (25) and bevel gear two (26) meshing connection, pivot two (27) one end and bevel gear two (26) fixed connection, pivot two (27) other end and bevel gear three (28) fixed connection, bevel gear three (28) are connected with actuating mechanism, pulley one (29) fixed mounting is on pivot two (27), pulley two (35) fixed mounting is on pivot three (30), and pulley one (29) and pulley two (35) are connected through first belt, pivot three (30) one end rotation is connected in cavity two (34) of pulley two (35), bevel gear two (30) are located, bevel gear two (27) one end is connected with bevel gear two (26) meshing connection, firing chamber (30) other end is connected with bevel gear three (30) fixed mounting has firing chamber (32) on the inner wall (60) fixed mounting has on pivot three inner wall (30), the bottom end of the burning chamber (60) is provided with a valve III (33).
8. A method for preparing silicon nitride powder by continuous ammonolysis as recited in claim 7, wherein the driving mechanism comprises: the motor (36), motor (36) fixed mounting is in cavity three (37) that processing case (22) set up, and the output shaft fixed mounting of motor (36) has gear three (38), gear three (38) and rack (39) meshing, rack (39) left side fixed mounting has slider (40), slider (40) from top to bottom sliding connection is in the spout that cavity three (37) set up, and fixed mounting has two-way driving motor (41) on rack (39), two-way driving motor (41) top output shaft and pivot four (42) one end non-fixed spline connection, pivot four (42) other end fixed mounting has bevel gear four (43), bevel gear four (43) and bevel gear three (28) meshing, two-way driving motor (41) bottom output shaft and worm (44) one end non-fixed spline connection, worm (44) other end swivelling joint is on cavity four (45) bottom inner wall, and fixedly mounting bevel gear five (46) on worm (44).
9. A method for preparing silicon nitride powder by continuous ammonolysis as claimed in claim 8, characterized in that the inside of the treatment tank (22) is also provided with a crushing mechanism comprising: the worm wheel (47), worm (47) meshes with worm (44) that establishes in the actuating mechanism, and install belt pulley III (48) on worm wheel (47) fixed mounting, drive roll (49) and driven voller (56) rotate respectively and connect on crushing room (50) inner wall, and drive roll (49) are connected through the second belt with driven voller (56) rear end, drive roll (49) front end fixed mounting has belt pulley IV (51), belt pulley III (48) are connected through the third belt with belt pulley IV (51), pivot V (52) one end and bevel gear V (53) fixed connection, pivot V (52) other end runs through crushing room (50) to rotate with crushing room (50) inner wall and be connected, and fixed mounting has a plurality of broken poles (54) on pivot V (52), bevel gear V (53) and bevel gear V (46) mesh, a plurality of broken balls (55) set up in crushing room (50).
10. A method for preparing silicon nitride powder by continuous ammonolysis as recited in claim 9, characterized in that a roasting chamber (57) is further provided in the processing box (22), the roasting chamber (57) is provided at the bottom end of the crushing chamber (50), one end of a connecting pipe six (58) is communicated with the crushing chamber (50), the other end of the connecting pipe six (58) is connected with the input end of the powder suction device (59), and the output end of the powder suction device (59) is communicated with the roasting chamber (57).
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