WO2024051305A1 - Production process and device for silicon nitride wave-absorbing material - Google Patents

Production process and device for silicon nitride wave-absorbing material Download PDF

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Publication number
WO2024051305A1
WO2024051305A1 PCT/CN2023/103526 CN2023103526W WO2024051305A1 WO 2024051305 A1 WO2024051305 A1 WO 2024051305A1 CN 2023103526 W CN2023103526 W CN 2023103526W WO 2024051305 A1 WO2024051305 A1 WO 2024051305A1
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Prior art keywords
shaft
crushing
silicon nitride
prefabricated tank
matching
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PCT/CN2023/103526
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French (fr)
Chinese (zh)
Inventor
肖亮
朱福林
曾小锋
许滔
钱利洪
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衡阳凯新特种材料科技有限公司
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Priority to GB2316480.9A priority Critical patent/GB2625432A/en
Publication of WO2024051305A1 publication Critical patent/WO2024051305A1/en

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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/78Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80Fibres, filaments, whiskers, platelets, or the like
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped 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
    • C04B35/58Shaped 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
    • C04B35/584Shaped 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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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/638Removal thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/444Halide containing anions, e.g. bromide, iodate, chlorite
    • CCHEMISTRY; METALLURGY
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52Constituents or additives characterised by their shapes
    • C04B2235/5208Fibers
    • C04B2235/5216Inorganic
    • C04B2235/524Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5248Carbon, e.g. graphite
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602Making the green bodies or pre-forms by moulding

Definitions

  • the invention relates to the technical field of stealth materials, specifically a production process and equipment of silicon nitride absorbing materials.
  • Nitride materials are expected to become a new type of absorbing application material due to their excellent physical and chemical properties.
  • the essence of absorbing waves is to absorb or attenuate incident electromagnetic waves, and convert the electromagnetic wave energy into heat energy or other forms of energy and dissipate it through the dielectric loss of the material.
  • Silicon nitride absorbing materials have the advantages of high temperature resistance, light weight, high strength, and good wave absorption performance, and have been researched very hotly in recent years.
  • Si/C/N absorbing materials not only have the above advantages, but also have a wide operating temperature range (can be used from room temperature to 1000°C), small dosage, adjustable dielectric properties, and can effectively weaken infrared radiation signals. Excellent characteristics. Most of the production processes of silicone absorbing materials are similar, roughly including ball milling, pulping, and sintering processes; however, ball milling and pulping cannot be carried out in an integrated manner, and the risk of intervention of interfering substances is greater.
  • the object of the present invention is to provide a production process and equipment for silicon nitride absorbing materials to solve the problems raised in the above background technology.
  • the present invention provides the following solutions:
  • a production process of silicon nitride wave absorbing material including the following steps:
  • Step 1 Prepare a premixed solvent, dissolve acrylamide and cross-linking agent in ethanol to prepare the premixed solvent, and adjust the pH of the solvent with ammonia water;
  • Step 2 Prepare dry powder, crush the silicon nitride matrix, ferric chloride particles, polymethyl methacrylate particles, carbon-based fibers, and alumina particles to make a powder and mix it for later use.
  • ferric chloride is used as silicon nitride.
  • Step 3 Prepare the substrate. Mix the powdery silicon nitride matrix, ferric chloride, polymethylmethacrylate, carbon-based fiber, and alumina with the premixed solvent. Add ferric chloride and polymethylmethacrylate. Under the action of ester, the components fuse and react with each other to form a colloidal base material;
  • Step 4 Material molding. Put the prepared base material into the mold for tape casting. After closing the mold, vacuum and dry at room temperature. After drying for 8 to 15 hours, the mold is demoulded to form a blank, and the blank is dry-pressed and degummed. remove organic matter from it;
  • Step 5 sintering, the degummed blank is placed in a nitrogen atmosphere for reaction sintering.
  • a powder-making assembly which includes a crushing drum fixed at the center of the upper layer inside the prefabricated tank through a No. 1 bracket, and a rolling compaction structure provided in the crushing drum; when the rolling compaction structure When rotating around the central axis of the crushing barrel, the particles in the crushing barrel can be crushed along the circumference; and the crushing force is positively correlated with the rotational speed of the crushing structure;
  • a homogeneous dispersion component is arranged in the prefabricated tank and mechanically cooperates with the rolling structure so that the dry powder crushed into powder and dropped into the prefabricated tank can be mixed with the prefabricated tank.
  • the premixed solvent in the tank is fully contacted and mixed for reaction.
  • the rolling structure includes a matching shaft that penetrates the center of the bottom of the crushing barrel and is sealed and rotatably connected with it, and a plurality of presses equidistantly distributed around the outer periphery of the matching shaft.
  • roller, and a pressure regulating mechanism provided on the matching shaft and connected to the pressure roller; when the matching shaft rotates, it can drive multiple pressure rollers to rotate around the matching shaft in the crushing barrel; and the pressure roller and the bottom of the crushing barrel Fitting, crushing the granular materials in the crushing cylinder; multiple filter holes are evenly opened at the bottom of the crushing cylinder.
  • a closed cavity is provided in the center of the interior of the matching shaft, and a built-in stepped shaft is movable inside the closed cavity;
  • the built-in stepped shaft is coaxial with the fitting shaft, and It can move along its axis in the closed cavity;
  • the pressure roller is rotatably connected to the built-in stepped shaft through a rotating shaft, and a second through groove connected to the closed cavity is provided on the matching shaft, and the rotating shaft passes through the second groove.
  • the through groove is rotatably connected to the built-in stepped shaft in the closed cavity;
  • the second through groove is opened parallel to the axis of the matching shaft, and the pressure regulating mechanism is connected to the built-in stepped shaft.
  • the pressure regulating mechanism includes a supporting plate fixed on the outer wall of the mating shaft along the circumference, a counterweight slidably arranged on the supporting plate, and a connecting The connecting rod between the counterweight block and the built-in stepped shaft; a first through groove connecting the upper part of the closed cavity is provided on the matching shaft; one end of the connecting rod is hinged with the counterweight block, and the other end is connected with the built-in stepped shaft.
  • the outer wall of the stepped shaft is hinged; wherein, the supporting plate is arranged along the radial direction of the fitting shaft, and the counterweight block is slidably arranged on the supporting plate along the radial direction of the fitting shaft.
  • the uniform dispersion assembly includes a driven shaft that is rotated in the center of the inside of the prefabricated tank, and the top of the driven shaft and the matching shaft run through the center of the bottom of the crushing barrel.
  • One end of the driven shaft is coaxially fixed; the bottom of the driven shaft is suspended in the prefabricated tank and close to the bottom of the prefabricated tank; there are multiple turns of torsion blades fixed at equal intervals along the circumference of the driven shaft.
  • a flange is provided in the center of the top of the top cover and connected to a reducer; the reducer is connected to the mating shaft through a transmission structure; the reducer has a A motor is installed on the side, and the rotor shaft of the motor is connected to the input end of the reducer.
  • the upper part of the matching shaft is provided with an upper chamber that penetrates the top of the matching shaft, and the inner wall of the upper chamber is provided with a keyway, and the keyway is parallel to the Match the axis of the shaft;
  • the transmission structure includes a transmission shaft connected to the output end of the reducer, and a key is installed on the lower outer wall of the transmission shaft, and the key is adapted to the keyway.
  • the lifting mechanism has a power cylinder and a A telescopic piece extends out of the power cylinder and telescopically cooperates with the power cylinder; the power cylinder is fixed to the prefabricated tank, and one end of the telescopic piece extends out of the power cylinder and is fixed to the lifting eye.
  • a solenoid valve is installed at the bottom of the prefabricated tank, and the solenoid valve cooperates with the discharge port opened in the center of the bottom of the prefabricated tank.
  • the powder-making and dispersion are synchronized and integrated, simplifying the procedures in the traditional preparation process; at the same time, compared with the mechanical forced crushing in the traditional process,
  • the rolling intensity in the present invention can match the rotation speed of the rolling structure, resulting in less wear and longer service life.
  • Can be used within a sealed container formed between the preformed can and top lid The preparation of dry powder, the preparation of premixed solvents, and the preparation of base materials are all carried out to prevent the intervention of external interfering substances.
  • Figure 1 is a schematic structural diagram of the production equipment of silicon nitride absorbing materials.
  • Figure 2 is another structural schematic diagram of production equipment for silicon nitride absorbing materials.
  • Figure 3 is a schematic structural diagram of the motor, reducer and top cover in the silicon nitride absorbing material production equipment.
  • Figure 4 is a schematic diagram of the internal structure of the silicon nitride absorbing material production equipment after the top cover is removed.
  • Figure 5 is a schematic structural diagram after removing the prefabricated tank based on Figure 4.
  • Figure 6 is a partial structural diagram of the crushing drum and matching shaft.
  • Figure 7 is a schematic structural diagram of Figure 6 from a reverse perspective.
  • Fig. 8 is a half-section schematic diagram of Fig. 7.
  • Figure 9 is a schematic structural diagram of Figure 6 after the crushing tube is removed.
  • Figure 10 is a schematic structural diagram after the built-in stepped shaft is removed from the closed cavity based on Figure 9.
  • Figure 11 is a half-section diagram of the mating shaft.
  • the purpose of the present invention is to provide a production process and equipment for silicon nitride absorbing materials to solve the problems existing in the existing technology.
  • the production process of silicon nitride absorbing material includes the following steps:
  • Step 1 Prepare a premixed solvent, dissolve acrylamide and cross-linking agent in ethanol to prepare the premixed solvent, and adjust the pH of the solvent with ammonia water;
  • Step 2 Prepare dry powder, crush the silicon nitride matrix, ferric chloride particles, polymethyl methacrylate particles, carbon-based fibers, and alumina particles to make a powder and mix it for later use.
  • ferric chloride is used as silicon nitride.
  • Step 3 Prepare the substrate. Mix the powdery silicon nitride matrix, ferric chloride, polymethylmethacrylate, carbon-based fiber, and alumina with the premixed solvent. Add ferric chloride and polymethylmethacrylate. Under the action of ester, the components fuse and react with each other to form a colloidal base material;
  • Step 4 Material molding. Put the prepared base material into the mold for tape casting. After closing the mold, vacuum and dry at room temperature. After drying for 8 to 15 hours, the mold is demoulded to form a blank, and the blank is dry-pressed and degummed. remove organic matter from it;
  • Step five sintering, place the degummed billet in a nitrogen atmosphere for reaction sintering, with a temperature of 1050 to 1200 degrees Celsius, a pressure of 500 to 800 MPa, and a sintering time of 4 to 5 hours.
  • the mechanical properties and wave-absorbing properties of the material are improved by adding carbon-based fibers, and the blank is shaped by the pressing process, and the various components are closely adhered to each other to avoid deformation during the sintering process; in addition, using Polymethylmethacrylate causes pores to form inside the substrate during the sintering process, increasing the porosity of the material, enhancing the impedance, and also reducing the reflectivity of the material;
  • the tape casting method is adopted so that the base material can be evenly distributed on the mold; the mold closing and vacuuming can prevent external interfering gas from hindering the development of the crystal phase of the material inside the base material, and sintering in a nitrogen atmosphere is more conducive to nitrogen
  • the growth of silicon crystals enhances the polarization loss of the molding material and improves the wave absorption performance.
  • the invention also provides a production equipment of silicon nitride absorbing material, which is used in the above process.
  • step one, step two, and step three the preparation of premixed solvent, the preparation of dry powder, and the preparation of base material.
  • the production equipment for silicon nitride absorbing materials includes a prefabricated tank 1 and a top cover 2 movable above the top of the prefabricated tank 1; the top cover 2 can seal the top of the prefabricated tank 1 Closed; when the top cover 2 tightly fits the top of the prefabricated can 1, a sealed container is formed between the prefabricated can 1 and the top cover 2.
  • dry powder preparation, premixed solvent preparation, and base material preparation can be carried out inside the container to prevent the intervention of external interfering substances.
  • the production equipment of silicon nitride absorbing materials also includes:
  • the milling assembly includes a crushing drum 8 fixed in the upper center of the interior of the prefabricated tank 1 through the No. 1 bracket 10, and a rolling structure arranged in the crushing drum 8; when the rolling structure rotates around the central axis of the crushing drum 8 When rotating, the particles in the crushing drum 8 can be crushed along the circumference; and the crushing intensity is positively correlated with the rotation speed of the crushing structure; the uniform dispersing component is arranged in the prefabricated tank 1 and is connected with the The rolling structure is mechanically coordinated so that the dry powder crushed into powder and dropped into the prefabricated tank 1 can fully contact the premixed solvent in the prefabricated tank 1 for mixing and reaction.
  • the crushing force in the present invention can match the rotation speed of the rolling structure; in comparison, traditional grinding equipment will crush the materials after the motor is started, especially when the motor has not reached the rated rotation speed. Since the crushing force cannot match the motor speed, the load on the motor is relatively large at the beginning of startup, and it is easy to burn the motor.
  • the rolling structure includes a mating shaft 9 that penetrates the center of the bottom of the crushing drum 8 and is sealed and rotatably connected with it, a plurality of pressure rollers 18 equidistantly distributed around the periphery of the mating shaft 9, and a plurality of pressure rollers 18 arranged on the mating shaft 9. And connected to the pressure regulating mechanism of the pressure roller 18; when the matching shaft 9 rotates, it can drive multiple pressure rollers 18 to rotate around the matching shaft 9 in the crushing barrel 8; and the pressure roller 18 is fit with the bottom of the crushing barrel 8, and the crushing barrel 8 The granular material inside is broken. Among them, a plurality of filter holes are evenly provided at the bottom of the crushing drum 8 .
  • the pressure regulating mechanism drives the pressure roller 18 to squeeze
  • the strength at the bottom of the crushing drum 8 increases accordingly, thereby increasing the crushing rate and allowing the input into the prefabricated tank
  • the amount of dry powder in 1 continues to increase; in addition, in the process of increasing the rotation speed of the matching shaft 9, the action rate of the homogeneous dispersion component mechanically matched with the rolling structure also increases, so that the amount of pre-processed powder is continuously increased and invested.
  • the dry powder in the can 1 can be mixed and reacted with the premixed solvent in a timely and effective manner.
  • a closed cavity 16 is provided in the center of the interior of the fitting shaft 9 , and a built-in stepped shaft 17 is movable inside the closed cavity 16 ; the built-in stepped shaft 17 is coaxial with the fitting shaft 9 , and can be moved in the closed cavity 16 The inside moves along its axis; the pressure roller 18 is rotatably connected to the built-in stepped shaft 17 through the rotating shaft.
  • the matching shaft 9 is provided with a second through groove 24 that communicates with the closed cavity 16. The rotating shaft passes through the second through groove 24 and the inside of the closed cavity 16.
  • the built-in stepped shaft 17 is rotatably connected; the second through groove 24 is opened parallel to the axis of the mating shaft 9, and the pressure regulating mechanism is connected to the built-in stepped shaft 17.
  • the rotation speed of the matching shaft 9 increases, the downward force exerted by the pressure regulating mechanism on the built-in stepped shaft 17 increases, and then the downward force transmitted to the pressure roller 18 through the rotating shaft increases, and finally the pressure roller 18 squeezes the crushing cylinder 8
  • the strength at the bottom increases accordingly.
  • extrusion force between the pressure roller 18 and the bottom of the crushing cylinder 8 in the present invention is a flexible force, which is different from the rigid force generated by mechanical connection in the prior art.
  • the pressure regulating mechanism includes a supporting plate 19 fixed circumferentially on the outer wall of the mating shaft 9, a counterweight 20 slidably disposed on the supporting plate 19, and a connecting weight 20 and a built-in stepped shaft 17.
  • the plate 19 is arranged along the radial direction of the fitting shaft 9
  • the counterweight 20 is slidably arranged on the supporting plate 19 along the radial direction of the fitting shaft 9 .
  • the supporting plate 19 is provided with a chute 22 that is slidably engaged with the lower part of the counterweight block 20 to prevent the counterweight block 20 from being detached from the supporting plate 19 .
  • the counterweight block 20 is detachably provided with a code block.
  • the code block is made of a material with a higher density, such as a lead block. Since the code block has a larger density, the corresponding weight is greater under the same volume.
  • the centrifugal force generated is greater; as the rotational speed of the mating shaft 9 increases, the rotational speed of the built-in stepped shaft 17 increases accordingly, thereby driving the counterweight 20 to rotate around the mating shaft 9.
  • the centrifugal force generated by the counterweight 20 drives the built-in stepped shaft 17 through the connecting rod 21 to have a downward tendency, thereby increasing the downward force of the pressure roller 18 and ultimately increasing the pressure roller 18 The breaking strength.
  • the squeezing force between the pressure roller 18 and the bottom of the crushing cylinder 8 in the present invention includes the downward force given by the built-in stepped shaft 17 and the self-weight of the pressure roller 18 .
  • the material of the code blocks can be adjusted according to actual production needs, such as copper blocks, iron blocks, lead blocks, etc.; the purpose of this setting is that by replacing the code blocks of different materials, the centrifugal force generated at the same speed will be different, resulting in the same
  • the squeezing force exerted by the pressing roller 18 is different at the rotating speed; it can be adjusted adaptively according to the softness and hardness of the material to be crushed.
  • lead blocks when breaking materials with higher hardness, lead blocks can be used; while for materials with lower hardness, iron blocks or copper blocks can be used.
  • the crushing force of the pressure roller 18 is mainly provided by the centrifugal force of the counterweight 20, the crushing force is a flexible force rather than a rigid force of mechanical connection.
  • centrifugal force is used to provide crushing force, which is a flexible force; if there is individual degeneration in the crushing cylinder 8
  • the pressure roller 18 in the present invention rolls the modified material for the first time, and the pressure can be reduced by lifting the pressure roller 18 to give way.
  • a flange is provided in the center of the top of the top cover 2 and is connected to a reducer; the reducer is connected to the mating shaft 9 through a transmission structure; a motor 4 is installed on one side of the reducer, and the rotor shaft of the motor 4 is connected The input end of the reducer.
  • the motor 4 outputs torque, and then outputs power to the transmission structure after being changed by the speed reducer, and finally the transmission structure drives the matching shaft 9 to rotate.
  • an upper chamber 15 that penetrates the top of the mating shaft 9 is provided on the upper part of the mating shaft 9.
  • a keyway 14 is formed on the inner wall of the upper chamber 15.
  • the keyway 14 is parallel to the axis of the mating shaft 9;
  • the transmission structure It includes a transmission shaft 6 connected to the output end of the reducer, and a key 7 is installed on the lower outer wall of the transmission shaft 6, and the key 7 is adapted to the keyway 14.
  • the transmission shaft 6 and the mating shaft 9 are connected through the cooperation of the key 7 and the keyway 14, so that the torque output by the motor 4 is transmitted to the transmission shaft 6 through the reducer, and finally drives the mating shaft 9 to rotate.
  • the edge of the top cover 2 is integrally provided with lifting lugs, and a lifting mechanism 3 is installed on the outer wall of the prefabricated tank 1.
  • the lifting mechanism 3 has a power cylinder and a power cylinder extending from the power cylinder. telescopic parts that telescopically cooperate with the power cylinder block; the power cylinder block and the prefabricated tank 1 are fixed Fixed, one end of the telescopic part extends out of the power cylinder body and is fixed with the lifting eye.
  • the power cylinder in the lifting mechanism 3 can drive the telescopic parts to expand and contract, thereby driving the lifting lugs and the top cover 2 to rise and fall, so that the top cover 2 can be separated and closed from the top of the prefabricated tank 1; when the top cover 2 and the top of the prefabricated tank 1 can be separated and closed; After the top opening of the prefabricated tank 1 is separated, the premixed solvent can be injected into the prefabricated tank 1; at the same time, granular materials can also be added to the crushing cylinder 8 in the prefabricated tank 1.
  • the homogeneous dispersion assembly includes a driven shaft 11 that is rotated and arranged in the center of the interior of the prefabricated tank 1.
  • the top of the driven shaft 11 and the matching shaft 9 are coaxially fixed with one end of the matching shaft 9 passing through the center of the bottom of the crushing drum 8;
  • the bottom of the driving shaft 11 is suspended in the prefabricated tank 1 and is close to the bottom of the prefabricated tank 1; a plurality of twisting blades 13 are fixed on the driven shaft 11 at equal intervals along the circumference.
  • two sets of No. 1 brackets 10 are fixed in the prefabricated tank 1.
  • bracket 10 has a through hole; the driven shaft 11 passes through the through hole and rotates with it; Two sets of flanges are provided on the driven shaft 11. Each set of flanges includes two rings of protrusions. The two rings of protrusions of the same set of flanges are respectively located on both sides of the through holes on the two sets of No. 1 brackets 10; using the through holes Keep the driven shaft 11 always located in the center of the prefabricated tank 1, and the flange provided prevents axial misalignment between the driven shaft 11 and the through hole.
  • the matching shaft 9 When the matching shaft 9 rotates, it can drive the driven shaft 11 to follow the synchronous rotation, thereby driving the twisting blade 13 to rotate, fully dispersing the premixed solvent and dry powder in the prefabricated tank 1, so that the dry powder of each component is evenly dissolved In premixed solvents, it accelerates the reaction and fusion between materials.
  • a solenoid valve 5 is installed at the bottom of the prefabricated tank 1, and the solenoid valve 5 cooperates with the discharge port opened in the center of the bottom of the prefabricated tank 1.
  • the solenoid valve 5 can be opened to allow the base material in the prefabricated tank 1 to flow out and be cast and discharged into the mold. .
  • the power cylinder in the lifting mechanism 3 drives the telescopic parts to expand and contract, thereby driving the lifting lugs and the top cover 2 to rise and fall, so that the top cover 2 and the top opening of the prefabricated tank 1 can be separated and closed; when the top cover 2 and the prefabricated tank 1 are After the top opening of the can 1 is separated, the premixed solvent can be injected into the prefabricated tank 1; at the same time, granular materials can also be added to the crushing cylinder 8 in the prefabricated tank 1
  • the transmission shaft 6 and the mating shaft 9 are connected by the cooperation of the key 7 and the keyway 14, driving the mating shaft 9 to rotate; the mating shaft 9 rotates
  • the built-in stepped shaft 17 is driven to follow the rotation, thereby driving the pressure roller 18 to rotate.
  • the built-in stepped shaft 17 rotates synchronously around the mating shaft 9; as the rotational speed of the mating shaft 9 increases, the rotational speed of the built-in stepped shaft 17 increases accordingly, thereby driving the counterweight 20 to rotate around the mating shaft 9.
  • centrifugal force is used to provide crushing force, which is a flexible force; if there is When some denatured raw materials have a higher hardness than normal materials and cannot be broken by one rolling, the pressure roller 18 in the present invention can crush the denatured material for the first time, and the pressure roller 18 can be lifted up to give way.
  • the matching shaft 9 When the matching shaft 9 rotates, it can drive the driven shaft 11 to follow the synchronous rotation, thereby driving the twisting blade 13 to rotate, fully dispersing the premixed solvent and dry powder in the prefabricated tank 1, so that the dry powder of each component is evenly dissolved In premixed solvents, it accelerates the reaction and fusion between materials.
  • the rotation speed of the driven shaft 11 that is mechanically connected to the matching shaft 9 also increases, so that the dry powder that is continuously increased and put into the prefabricated tank 1 can be mixed with the preform in a timely and effective manner. Solvent mixing reaction.

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Abstract

The present invention relates to a process technology and device, specifically a production process and device for a silicon nitride wave-absorbing material. The production process comprises preparing a premixed solvent, preparing dry powder, preparing a base material, forming the material, and sintering. By means of the device in the present invention, preparation of the dry powder, preparation of the premixed solvent, and preparation of the base material are carried out in a sealed container, and intervention of external interfering substances is avoided. The device in the present invention comprises a powder preparation assembly and a uniform dispersion assembly. When a rolling structure rotates around the central axis of a crushing barrel, the rolling structure can press and grind particles in the crushing barrel along the circumference; the pressing and grinding force is in a positive correlation with the rotation speed of the rolling structure; powder preparation and dispersion are synchronously and integrally carried out, and the procedures in a conventional preparation process are simplified. Moreover, compared with mechanical forced crushing in a conventional process, in the present invention, the pressing and grinding force can be matched with the rotation peed of the rolling structure, abrasion is smaller, and the service life is longer.

Description

一种氮化硅吸波材料的生产工艺及设备A kind of production technology and equipment of silicon nitride wave absorbing material 技术领域Technical field
本发明涉及隐身材料技术领域,具体是一种氮化硅吸波材料的生产工艺及设备。The invention relates to the technical field of stealth materials, specifically a production process and equipment of silicon nitride absorbing materials.
背景技术Background technique
隐身材料对提高武器装备的生存和防御能力具有重要意义。氮化物材料由于其自身优异的物理化学性能,有望成为一种新型吸波应用材料。吸波材料的吸波实质是吸收或衰减入射的电磁波,并通过材料的介质损耗使电磁波能量转变成热能或其它形式的能量而耗散掉。而氮化硅吸波材料具有耐高温、质量轻、强度大、吸波性能好等优点,近年来研究热度十分高。尤其是Si/C/N吸波材料,不仅具有以上优点,还具有使用温度范围宽(从室温到1000℃均可使用)、用量小、介电性能可调、可以有效地减弱红外辐射信号的优良特性。化硅吸波材料的生产大多工艺相似,大致为球磨、制浆、烧结工序;但是球磨和制浆之间无法做到一体进行,干扰物质的介入风险较大。Stealth materials are of great significance to improving the survivability and defense capabilities of weapons and equipment. Nitride materials are expected to become a new type of absorbing application material due to their excellent physical and chemical properties. The essence of absorbing waves is to absorb or attenuate incident electromagnetic waves, and convert the electromagnetic wave energy into heat energy or other forms of energy and dissipate it through the dielectric loss of the material. Silicon nitride absorbing materials have the advantages of high temperature resistance, light weight, high strength, and good wave absorption performance, and have been researched very hotly in recent years. In particular, Si/C/N absorbing materials not only have the above advantages, but also have a wide operating temperature range (can be used from room temperature to 1000°C), small dosage, adjustable dielectric properties, and can effectively weaken infrared radiation signals. Excellent characteristics. Most of the production processes of silicone absorbing materials are similar, roughly including ball milling, pulping, and sintering processes; however, ball milling and pulping cannot be carried out in an integrated manner, and the risk of intervention of interfering substances is greater.
发明内容Contents of the invention
本发明的目的在于提供一种氮化硅吸波材料的生产工艺及设备,以解决上述背景技术中提出的问题。The object of the present invention is to provide a production process and equipment for silicon nitride absorbing materials to solve the problems raised in the above background technology.
为实现上述目的,本发明提供了如下方案:In order to achieve the above objects, the present invention provides the following solutions:
一种氮化硅吸波材料的生产工艺,包括如下步骤:A production process of silicon nitride wave absorbing material, including the following steps:
步骤一,配制预混溶剂,将丙烯酰胺和交联剂溶于乙醇中制备预混溶剂,并用氨水调剂溶剂的pH;Step 1: Prepare a premixed solvent, dissolve acrylamide and cross-linking agent in ethanol to prepare the premixed solvent, and adjust the pH of the solvent with ammonia water;
步骤二,预备干粉,对氮化硅基体、氯化铁颗粒、聚甲基丙烯酸甲酯颗粒、碳基纤维、以及氧化铝颗粒破碎,制成粉末混合备用,其中,氯化铁作为氮化硅吸波材料生产的催化剂使用;Step 2: Prepare dry powder, crush the silicon nitride matrix, ferric chloride particles, polymethyl methacrylate particles, carbon-based fibers, and alumina particles to make a powder and mix it for later use. Among them, ferric chloride is used as silicon nitride. Use of catalysts in the production of absorbing materials;
步骤三,基材制备,将粉状的氮化硅基体、氯化铁、聚甲基丙烯酸甲酯、碳基纤维、以及氧化铝同预混溶剂混合,在氯化铁和聚甲基丙烯酸甲 酯的作用下使各组分相互融合反应,生成胶状基材;Step 3: Prepare the substrate. Mix the powdery silicon nitride matrix, ferric chloride, polymethylmethacrylate, carbon-based fiber, and alumina with the premixed solvent. Add ferric chloride and polymethylmethacrylate. Under the action of ester, the components fuse and react with each other to form a colloidal base material;
步骤四,材料成型,将制备的基材排入到模具中流延成型,合模后抽真空,于常温下干燥;干燥8~15小时后脱模形成坯材,并对坯材干压脱胶,去除其中的有机物;Step 4: Material molding. Put the prepared base material into the mold for tape casting. After closing the mold, vacuum and dry at room temperature. After drying for 8 to 15 hours, the mold is demoulded to form a blank, and the blank is dry-pressed and degummed. remove organic matter from it;
步骤五,烧结,将脱胶后的坯材置于氮气氛围下反应烧结。Step 5: sintering, the degummed blank is placed in a nitrogen atmosphere for reaction sintering.
一种适用于上述工艺的氮化硅吸波材料生产设备,用于在氮化硅吸波材料的生产工艺中,配制预混溶剂、预备干粉、以及制备基材;包括预制罐和活动设置在所述预制罐顶口上方的顶盖;所述顶盖可将预制罐的顶口封闭;当顶盖严密贴合预制罐的顶口时,预制罐和顶盖之间形成一个密封容器;A silicon nitride absorbing material production equipment suitable for the above process, used for preparing premixed solvents, preparing dry powder, and preparing base materials in the production process of silicon nitride absorbing materials; including prefabricated tanks and movable settings A top cover above the top opening of the prefabricated tank; the top cover can seal the top opening of the prefabricated tank; when the top cover tightly fits the top opening of the prefabricated tank, a formation is formed between the prefabricated tank and the top cover a sealed container;
还包括:制粉组件,所述制粉组件包括通过一号支架固定在所述预制罐内部上层中央的破碎筒,以及设置在所述破碎筒内的碾压结构;当所述碾压结构绕所述破碎筒的中心轴线转动时,可沿圆周对破碎筒内的颗粒物进行压碾;且压碾力度同碾压结构的转速呈正相关关系;It also includes: a powder-making assembly, which includes a crushing drum fixed at the center of the upper layer inside the prefabricated tank through a No. 1 bracket, and a rolling compaction structure provided in the crushing drum; when the rolling compaction structure When rotating around the central axis of the crushing barrel, the particles in the crushing barrel can be crushed along the circumference; and the crushing force is positively correlated with the rotational speed of the crushing structure;
均置分散组件,所述均置分散组件设置于所述预制罐内,并与所述碾压结构机械配合,以使压碾成粉并掉落至预制罐内的干粉能够与预制罐内的预混溶剂充分接触,混合反应。A homogeneous dispersion component is arranged in the prefabricated tank and mechanically cooperates with the rolling structure so that the dry powder crushed into powder and dropped into the prefabricated tank can be mixed with the prefabricated tank. The premixed solvent in the tank is fully contacted and mixed for reaction.
如上所述的氮化硅吸波材料的生产设备:所述碾压结构包括贯穿所述破碎筒底部中央并与之密封转动连接的配合轴、等距分布在所述配合轴外周的多个压辊、以及设置在所述配合轴上并连接所述压辊的调压机构;当所述配合轴旋转时可带动多个压辊在破碎筒内绕配合轴旋转;且压辊与破碎筒底部贴合,对破碎筒内的颗粒材料破碎;在所述破碎筒的底部均匀开设有多个滤孔。The production equipment of silicon nitride absorbing material as described above: the rolling structure includes a matching shaft that penetrates the center of the bottom of the crushing barrel and is sealed and rotatably connected with it, and a plurality of presses equidistantly distributed around the outer periphery of the matching shaft. roller, and a pressure regulating mechanism provided on the matching shaft and connected to the pressure roller; when the matching shaft rotates, it can drive multiple pressure rollers to rotate around the matching shaft in the crushing barrel; and the pressure roller and the bottom of the crushing barrel Fitting, crushing the granular materials in the crushing cylinder; multiple filter holes are evenly opened at the bottom of the crushing cylinder.
如上所述的氮化硅吸波材料的生产设备:所述配合轴的内部中央设置有封闭腔,封闭腔内活动设置有内置阶梯轴;所述内置阶梯轴与所述配合轴同轴,且其可在封闭腔内沿其轴线活动;所述压辊通过转轴与内置阶梯轴转动连接,在所述配合轴上开设有连通所述封闭腔的第二穿槽,所述转轴穿过第二穿槽与封闭腔内的内置阶梯轴转动连接;所述第二穿槽平行于所述配合轴的轴线开设,调压机构连接所述内置阶梯轴。 The production equipment of silicon nitride absorbing material as described above: a closed cavity is provided in the center of the interior of the matching shaft, and a built-in stepped shaft is movable inside the closed cavity; the built-in stepped shaft is coaxial with the fitting shaft, and It can move along its axis in the closed cavity; the pressure roller is rotatably connected to the built-in stepped shaft through a rotating shaft, and a second through groove connected to the closed cavity is provided on the matching shaft, and the rotating shaft passes through the second groove. The through groove is rotatably connected to the built-in stepped shaft in the closed cavity; the second through groove is opened parallel to the axis of the matching shaft, and the pressure regulating mechanism is connected to the built-in stepped shaft.
如上所述的氮化硅吸波材料的生产设备:所述调压机构包括沿圆周固定在所述配合轴外壁上的托板、滑动设置在所述托板上的配重块、以及连接所述配重块与所述内置阶梯轴的连杆;在所述配合轴上开设有连通所述封闭腔上部的第一穿槽;连杆的一端与所述配重块铰接,另一端与内置阶梯轴的外壁铰接;其中,所述托板沿所述配合轴的径向设置,配重块沿所述配合轴的径向滑动设置在所述托板上。The production equipment of silicon nitride absorbing material as described above: the pressure regulating mechanism includes a supporting plate fixed on the outer wall of the mating shaft along the circumference, a counterweight slidably arranged on the supporting plate, and a connecting The connecting rod between the counterweight block and the built-in stepped shaft; a first through groove connecting the upper part of the closed cavity is provided on the matching shaft; one end of the connecting rod is hinged with the counterweight block, and the other end is connected with the built-in stepped shaft. The outer wall of the stepped shaft is hinged; wherein, the supporting plate is arranged along the radial direction of the fitting shaft, and the counterweight block is slidably arranged on the supporting plate along the radial direction of the fitting shaft.
如上所述的氮化硅吸波材料的生产设备:所述均置分散组件包括转动设置在所述预制罐内部中央的从动轴,所述从动轴顶部与配合轴贯穿破碎筒底部中央的一端同轴固定;从动轴的底部悬空于所述预制罐内并接近预制罐的底部;从动轴上沿圆周等距固定有多圈扭转叶片。The production equipment of silicon nitride absorbing material as described above: the uniform dispersion assembly includes a driven shaft that is rotated in the center of the inside of the prefabricated tank, and the top of the driven shaft and the matching shaft run through the center of the bottom of the crushing barrel. One end of the driven shaft is coaxially fixed; the bottom of the driven shaft is suspended in the prefabricated tank and close to the bottom of the prefabricated tank; there are multiple turns of torsion blades fixed at equal intervals along the circumference of the driven shaft.
如上所述的氮化硅吸波材料的生产设备:所述顶盖的顶部中央设置有法兰,并连接减速器;所述减速器通过传动结构与所述配合轴连接;所述减速器一侧安装有马达,所述马达的转子轴连接减速器的输入端。The production equipment of silicon nitride absorbing material as described above: a flange is provided in the center of the top of the top cover and connected to a reducer; the reducer is connected to the mating shaft through a transmission structure; the reducer has a A motor is installed on the side, and the rotor shaft of the motor is connected to the input end of the reducer.
如上所述的氮化硅吸波材料的生产设备:所述配合轴的上部开设有贯通所述配合轴顶部的上腔室,所述上腔室的内壁上开设有键槽,键槽平行于所述配合轴的轴线;所述传动结构包括连接所述减速器输出端的传动轴,所述传动轴的下部外壁安装有卡键,所述卡键与所述键槽适配。The production equipment of silicon nitride absorbing material as mentioned above: the upper part of the matching shaft is provided with an upper chamber that penetrates the top of the matching shaft, and the inner wall of the upper chamber is provided with a keyway, and the keyway is parallel to the Match the axis of the shaft; the transmission structure includes a transmission shaft connected to the output end of the reducer, and a key is installed on the lower outer wall of the transmission shaft, and the key is adapted to the keyway.
如上所述的氮化硅吸波材料的生产设备:所述顶盖的边缘一体设置有吊耳,在预制罐的外壁上安装有顶升机构,所述顶升机构具有一个动力缸体和一个伸出于所述动力缸体并与动力缸体伸缩配合的伸缩件;所述动力缸体与预制罐固定,伸缩件伸出所述动力缸体的一端与吊耳固定。The silicon nitride absorbing material production equipment as described above: the edge of the top cover is integrally provided with lifting lugs, and a lifting mechanism is installed on the outer wall of the prefabricated tank. The lifting mechanism has a power cylinder and a A telescopic piece extends out of the power cylinder and telescopically cooperates with the power cylinder; the power cylinder is fixed to the prefabricated tank, and one end of the telescopic piece extends out of the power cylinder and is fixed to the lifting eye.
如上所述的氮化硅吸波材料的生产设备:所述预制罐的底部安装有电磁阀,所述电磁阀与开设于所述预制罐底部中央的排放口配合。The production equipment of silicon nitride absorbing material as described above: a solenoid valve is installed at the bottom of the prefabricated tank, and the solenoid valve cooperates with the discharge port opened in the center of the bottom of the prefabricated tank.
与现有技术相比,本发明的有益效果是:Compared with the prior art, the beneficial effects of the present invention are:
通过将制粉组件中的碾压结构与均置分散组件机械连接,实现制粉与分散同步一体进行,简化了传统的制备工艺中的工序;同时,相较于传统工艺中的机械强制破碎而言,本发明中的压碾力度可与碾压结构的转速匹配,磨损更小,使用寿命更长。可在预制罐和顶盖之间形成的密封容器内 部进行干粉的预备、预混溶剂的配制、以及基材的制备,杜绝外界干扰性物质介入。By mechanically connecting the rolling structure in the powder-making component with the homogeneous dispersion component, the powder-making and dispersion are synchronized and integrated, simplifying the procedures in the traditional preparation process; at the same time, compared with the mechanical forced crushing in the traditional process, In other words, the rolling intensity in the present invention can match the rotation speed of the rolling structure, resulting in less wear and longer service life. Can be used within a sealed container formed between the preformed can and top lid The preparation of dry powder, the preparation of premixed solvents, and the preparation of base materials are all carried out to prevent the intervention of external interfering substances.
附图说明Description of the drawings
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。In order to explain the embodiments of the present invention or the technical solutions in the prior art more clearly, the drawings needed to be used in the embodiments will be briefly introduced below. Obviously, the drawings in the following description are only some of the drawings of the present invention. Embodiments, for those of ordinary skill in the art, other drawings can also be obtained based on these drawings without exerting creative efforts.
图1为氮化硅吸波材料的生产设备的结构示意图。Figure 1 is a schematic structural diagram of the production equipment of silicon nitride absorbing materials.
图2为氮化硅吸波材料的生产设备的又一结构示意图。Figure 2 is another structural schematic diagram of production equipment for silicon nitride absorbing materials.
图3为氮化硅吸波材料的生产设备中马达和减速器以及顶盖的结构示意图。Figure 3 is a schematic structural diagram of the motor, reducer and top cover in the silicon nitride absorbing material production equipment.
图4为拆除顶盖后的氮化硅吸波材料的生产设备的内部结构示意图。Figure 4 is a schematic diagram of the internal structure of the silicon nitride absorbing material production equipment after the top cover is removed.
图5为在图4的基础上拆除预制罐后的结构示意图。Figure 5 is a schematic structural diagram after removing the prefabricated tank based on Figure 4.
图6为破碎筒和配合轴的局部结构示意图。Figure 6 is a partial structural diagram of the crushing drum and matching shaft.
图7为图6反向视角的的结构示意图。Figure 7 is a schematic structural diagram of Figure 6 from a reverse perspective.
图8为图7的半剖示意图。Fig. 8 is a half-section schematic diagram of Fig. 7.
图9为图6中拆除破碎筒后的结构示意图。Figure 9 is a schematic structural diagram of Figure 6 after the crushing tube is removed.
图10为在图9的基础上将内置阶梯轴从封闭腔中拆出后的结构示意图。Figure 10 is a schematic structural diagram after the built-in stepped shaft is removed from the closed cavity based on Figure 9.
图11为配合轴的半剖示意图。Figure 11 is a half-section diagram of the mating shaft.
图中:1-预制罐;2-顶盖;3-顶升机构;4-马达;5-电磁阀;6-传动轴;7-卡键;8-破碎筒;9-配合轴;10-一号支架;11-从动轴;12-二号支架;13-扭转叶片;14-键槽;15-上腔室;16-封闭腔;17-内置阶梯轴;18-压辊;19-托板;20-配重块;21-连杆;22-滑槽;23-第一穿槽;24-第二穿槽。In the picture: 1-prefabricated tank; 2-top cover; 3-jacking mechanism; 4-motor; 5-solenoid valve; 6-drive shaft; 7-key; 8-breaking barrel; 9-fitting shaft; 10 -No.1 bracket; 11-driven shaft; 12-No.2 bracket; 13-torsion blade; 14-keyway; 15-upper chamber; 16-closed chamber; 17-built-in stepped shaft; 18-pressure roller; 19- Supporting plate; 20-counterweight block; 21-connecting rod; 22-slide; 23-first through groove; 24-second through groove.
具体实施方式Detailed ways
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没 有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, those of ordinary skill in the art will not All other embodiments obtained by making creative efforts belong to the scope of protection of the present invention.
本发明的目的是提供一种氮化硅吸波材料的生产工艺及设备,以解决现有技术存在的问题。The purpose of the present invention is to provide a production process and equipment for silicon nitride absorbing materials to solve the problems existing in the existing technology.
为使本发明的上述目的、特征和优点能够更加明显易懂,下面结合附图和具体实施方式对本发明作进一步详细的说明。In order to make the above objects, features and advantages of the present invention more obvious and understandable, the present invention will be described in further detail below with reference to the accompanying drawings and specific embodiments.
作为本发明的一种实施例,所述氮化硅吸波材料的生产工艺,包括如下步骤:As an embodiment of the present invention, the production process of silicon nitride absorbing material includes the following steps:
步骤一,配制预混溶剂,将丙烯酰胺和交联剂溶于乙醇中制备预混溶剂,并用氨水调剂溶剂的pH;Step 1: Prepare a premixed solvent, dissolve acrylamide and cross-linking agent in ethanol to prepare the premixed solvent, and adjust the pH of the solvent with ammonia water;
步骤二,预备干粉,对氮化硅基体、氯化铁颗粒、聚甲基丙烯酸甲酯颗粒、碳基纤维、以及氧化铝颗粒破碎,制成粉末混合备用,其中,氯化铁作为氮化硅吸波材料生产的催化剂使用;Step 2: Prepare dry powder, crush the silicon nitride matrix, ferric chloride particles, polymethyl methacrylate particles, carbon-based fibers, and alumina particles to make a powder and mix it for later use. Among them, ferric chloride is used as silicon nitride. Use of catalysts in the production of absorbing materials;
步骤三,基材制备,将粉状的氮化硅基体、氯化铁、聚甲基丙烯酸甲酯、碳基纤维、以及氧化铝同预混溶剂混合,在氯化铁和聚甲基丙烯酸甲酯的作用下使各组分相互融合反应,生成胶状基材;Step 3: Prepare the substrate. Mix the powdery silicon nitride matrix, ferric chloride, polymethylmethacrylate, carbon-based fiber, and alumina with the premixed solvent. Add ferric chloride and polymethylmethacrylate. Under the action of ester, the components fuse and react with each other to form a colloidal base material;
步骤四,材料成型,将制备的基材排入到模具中流延成型,合模后抽真空,于常温下干燥;干燥8~15小时后脱模形成坯材,并对坯材干压脱胶,去除其中的有机物;Step 4: Material molding. Put the prepared base material into the mold for tape casting. After closing the mold, vacuum and dry at room temperature. After drying for 8 to 15 hours, the mold is demoulded to form a blank, and the blank is dry-pressed and degummed. remove organic matter from it;
步骤五,烧结,将脱胶后的坯材置于氮气氛围下反应烧结,温度为1050~1200摄氏度,压强为500~800MPa,烧结时长4~5小时。Step five, sintering, place the degummed billet in a nitrogen atmosphere for reaction sintering, with a temperature of 1050 to 1200 degrees Celsius, a pressure of 500 to 800 MPa, and a sintering time of 4 to 5 hours.
本发明的工艺中,通过增加碳基纤维提高材料的力学性能及吸波性能,借助压制工艺使坯材成型,各个组分之间紧密贴合,避免在烧结的过程中产生变形;此外,利用聚甲基丙烯酸甲酯使基材在烧结的过程中内部形成气孔,提升材料的孔隙率,增强阻抗,同时还降低了材料的反射率;In the process of the present invention, the mechanical properties and wave-absorbing properties of the material are improved by adding carbon-based fibers, and the blank is shaped by the pressing process, and the various components are closely adhered to each other to avoid deformation during the sintering process; in addition, using Polymethylmethacrylate causes pores to form inside the substrate during the sintering process, increasing the porosity of the material, enhancing the impedance, and also reducing the reflectivity of the material;
本发明的工艺中,采用流延成型的方式使得基材能够均匀地分布在模具上;合模抽真空可避免外界干扰气体阻碍基材内部材料的晶相发育,氮气氛围下烧结更有利于氮化硅结晶的生长,增强成型材料的极化损耗,提高吸波性能。In the process of the present invention, the tape casting method is adopted so that the base material can be evenly distributed on the mold; the mold closing and vacuuming can prevent external interfering gas from hindering the development of the crystal phase of the material inside the base material, and sintering in a nitrogen atmosphere is more conducive to nitrogen The growth of silicon crystals enhances the polarization loss of the molding material and improves the wave absorption performance.
本发明还提供了一种氮化硅吸波材料的生产设备,用于在上述工艺的 步骤一、步骤二、以及步骤三中,预混溶剂的配制、干粉的预备、以及基材制备。The invention also provides a production equipment of silicon nitride absorbing material, which is used in the above process. In step one, step two, and step three, the preparation of premixed solvent, the preparation of dry powder, and the preparation of base material.
请参阅图1~图11,氮化硅吸波材料的生产设备包括预制罐1和活动设置在预制罐1顶口上方的顶盖2;顶盖2可将预制罐1的顶口封闭;当顶盖2严密贴合预制罐1的顶口时,预制罐1和顶盖2之间形成一个密封容器。Please refer to Figures 1 to 11. The production equipment for silicon nitride absorbing materials includes a prefabricated tank 1 and a top cover 2 movable above the top of the prefabricated tank 1; the top cover 2 can seal the top of the prefabricated tank 1 Closed; when the top cover 2 tightly fits the top of the prefabricated can 1, a sealed container is formed between the prefabricated can 1 and the top cover 2.
借助预制罐1和顶盖2形成的密封容器,可在该容器内部进行干粉的预备、预混溶剂的配制、以及基材的制备,杜绝外界干扰性物质介入。With the help of the sealed container formed by the prefabricated tank 1 and the top cover 2, dry powder preparation, premixed solvent preparation, and base material preparation can be carried out inside the container to prevent the intervention of external interfering substances.
氮化硅吸波材料的生产设备还包括:The production equipment of silicon nitride absorbing materials also includes:
制粉组件,制粉组件包括通过一号支架10固定在预制罐1内部上层中央的破碎筒8,以及设置在破碎筒8内的碾压结构;当碾压结构绕破碎筒8的中心轴线转动时,可沿圆周对破碎筒8内的颗粒物进行压碾;且压碾力度同碾压结构的转速呈正相关关系;均置分散组件,均置分散组件设置于预制罐1内,并与碾压结构机械配合,以使压碾成粉并掉落至预制罐1内的干粉能够与预制罐1内的预混溶剂充分接触,混合反应。The milling assembly includes a crushing drum 8 fixed in the upper center of the interior of the prefabricated tank 1 through the No. 1 bracket 10, and a rolling structure arranged in the crushing drum 8; when the rolling structure rotates around the central axis of the crushing drum 8 When rotating, the particles in the crushing drum 8 can be crushed along the circumference; and the crushing intensity is positively correlated with the rotation speed of the crushing structure; the uniform dispersing component is arranged in the prefabricated tank 1 and is connected with the The rolling structure is mechanically coordinated so that the dry powder crushed into powder and dropped into the prefabricated tank 1 can fully contact the premixed solvent in the prefabricated tank 1 for mixing and reaction.
本发明中,通过将制粉组件中的碾压结构与均置分散组件机械连接,实现制粉与分散同步一体进行,简化了传统的制备工艺中的工序;同时,相较于传统工艺中的机械强制破碎而言,本发明中的压碾力度可与碾压结构的转速匹配;作为对比,传统的研磨设备在电机启动后便会对物料进行破碎,尤其时在电机尚未达到额定转速时,由于压碾的力度不能够匹配电机转速,导致电机启动之初的负载较大,极易烧毁电机。In the present invention, by mechanically connecting the rolling structure in the powder-making assembly with the homogeneous dispersion assembly, powder-making and dispersion are synchronized and integrated, simplifying the procedures in the traditional preparation process; at the same time, compared with the traditional process, For mechanical forced crushing, the crushing force in the present invention can match the rotation speed of the rolling structure; in comparison, traditional grinding equipment will crush the materials after the motor is started, especially when the motor has not reached the rated rotation speed. Since the crushing force cannot match the motor speed, the load on the motor is relatively large at the beginning of startup, and it is easy to burn the motor.
作为本发明进一步的方案,碾压结构包括贯穿破碎筒8底部中央并与之密封转动连接的配合轴9、等距分布在配合轴9外周的多个压辊18、以及设置在配合轴9上并连接压辊18的调压机构;当配合轴9旋转时可带动多个压辊18在破碎筒8内绕配合轴9旋转;且压辊18与破碎筒8底部贴合,对破碎筒8内的颗粒材料破碎。其中,在破碎筒8的底部均匀开设有多个滤孔。As a further solution of the present invention, the rolling structure includes a mating shaft 9 that penetrates the center of the bottom of the crushing drum 8 and is sealed and rotatably connected with it, a plurality of pressure rollers 18 equidistantly distributed around the periphery of the mating shaft 9, and a plurality of pressure rollers 18 arranged on the mating shaft 9. And connected to the pressure regulating mechanism of the pressure roller 18; when the matching shaft 9 rotates, it can drive multiple pressure rollers 18 to rotate around the matching shaft 9 in the crushing barrel 8; and the pressure roller 18 is fit with the bottom of the crushing barrel 8, and the crushing barrel 8 The granular material inside is broken. Among them, a plurality of filter holes are evenly provided at the bottom of the crushing drum 8 .
颗粒材料破碎程度达到成粉状,且粉径小于滤孔的直径时,通过滤孔排入到预制罐1内;随着配合轴9的转速增大,调压机构驱使压辊18挤压破碎筒8底部的力度相应增大,从而提高破碎速率,使得投入到预制罐 1内的干粉量不断增大;另外,在配合轴9的转速增大的过程中,与碾压结构机械配合的均置分散组件的动作速率也随之增大,使得不断增加并投入到预制罐1内的干粉能够及时有效地与预混溶剂混合反应。When the granular material is broken into powder and the powder diameter is smaller than the diameter of the filter hole, it is discharged into the prefabricated tank 1 through the filter hole; as the rotation speed of the matching shaft 9 increases, the pressure regulating mechanism drives the pressure roller 18 to squeeze The strength at the bottom of the crushing drum 8 increases accordingly, thereby increasing the crushing rate and allowing the input into the prefabricated tank The amount of dry powder in 1 continues to increase; in addition, in the process of increasing the rotation speed of the matching shaft 9, the action rate of the homogeneous dispersion component mechanically matched with the rolling structure also increases, so that the amount of pre-processed powder is continuously increased and invested. The dry powder in the can 1 can be mixed and reacted with the premixed solvent in a timely and effective manner.
作为本发明更进一步的方案,配合轴9的内部中央设置有封闭腔16,封闭腔16内活动设置有内置阶梯轴17;内置阶梯轴17与配合轴9同轴,且其可在封闭腔16内沿其轴线活动;压辊18通过转轴与内置阶梯轴17转动连接,在配合轴9上开设有连通封闭腔16的第二穿槽24,转轴穿过第二穿槽24与封闭腔16内的内置阶梯轴17转动连接;第二穿槽24平行于配合轴9的轴线开设,调压机构连接内置阶梯轴17。随着配合轴9的转速增大,使得调压机构向内置阶梯轴17施加的下压力增大,进而通过转轴传递到压辊18的下压力增大,最终使压辊18挤压破碎筒8底部的力度相应增大。As a further solution of the present invention, a closed cavity 16 is provided in the center of the interior of the fitting shaft 9 , and a built-in stepped shaft 17 is movable inside the closed cavity 16 ; the built-in stepped shaft 17 is coaxial with the fitting shaft 9 , and can be moved in the closed cavity 16 The inside moves along its axis; the pressure roller 18 is rotatably connected to the built-in stepped shaft 17 through the rotating shaft. The matching shaft 9 is provided with a second through groove 24 that communicates with the closed cavity 16. The rotating shaft passes through the second through groove 24 and the inside of the closed cavity 16. The built-in stepped shaft 17 is rotatably connected; the second through groove 24 is opened parallel to the axis of the mating shaft 9, and the pressure regulating mechanism is connected to the built-in stepped shaft 17. As the rotation speed of the matching shaft 9 increases, the downward force exerted by the pressure regulating mechanism on the built-in stepped shaft 17 increases, and then the downward force transmitted to the pressure roller 18 through the rotating shaft increases, and finally the pressure roller 18 squeezes the crushing cylinder 8 The strength at the bottom increases accordingly.
注意的是,本发明中的压辊18与破碎筒8底部之间的挤压力为柔性力,区别于现有技术中通过机械连接所产生的刚性力。It should be noted that the extrusion force between the pressure roller 18 and the bottom of the crushing cylinder 8 in the present invention is a flexible force, which is different from the rigid force generated by mechanical connection in the prior art.
作为本发明再进一步的方案,调压机构包括沿圆周固定在配合轴9外壁上的托板19、滑动设置在托板19上的配重块20、以及连接配重块20与内置阶梯轴17的连杆21;在配合轴9上开设有连通封闭腔16上部的第一穿槽23;连杆21的一端与配重块20铰接,另一端与内置阶梯轴17的外壁铰接;其中,托板19沿配合轴9的径向设置,配重块20沿配合轴9的径向滑动设置在托板19上。在托板19上开设有同配重块20的下部滑动嵌合的滑槽22,以避免配重块20从托板19上脱离。As a further solution of the present invention, the pressure regulating mechanism includes a supporting plate 19 fixed circumferentially on the outer wall of the mating shaft 9, a counterweight 20 slidably disposed on the supporting plate 19, and a connecting weight 20 and a built-in stepped shaft 17. The connecting rod 21; a first through groove 23 connected to the upper part of the closed cavity 16 is provided on the matching shaft 9; one end of the connecting rod 21 is hinged with the counterweight 20, and the other end is hinged with the outer wall of the built-in ladder shaft 17; wherein, the support The plate 19 is arranged along the radial direction of the fitting shaft 9 , and the counterweight 20 is slidably arranged on the supporting plate 19 along the radial direction of the fitting shaft 9 . The supporting plate 19 is provided with a chute 22 that is slidably engaged with the lower part of the counterweight block 20 to prevent the counterweight block 20 from being detached from the supporting plate 19 .
配重块20上可拆卸设置有码块,码块采用密度较大的材料所制,例如铅块;由于码块的密度较大,因此,在相同体积下,对应的重量更大;在其绕配合轴9转动时,所产生的离心力更大;随着配合轴9的转速增大,使得内置阶梯轴17的转速跟随增大,从而带动配重块20绕配合轴9旋转的转速增大,导致配重块20产生的离心力增大;配重块20产生的离心力通过连杆21带动内置阶梯轴17具有下压的趋势,从而使得压辊18的下压力增大,最终提高压辊18的破碎力度。The counterweight block 20 is detachably provided with a code block. The code block is made of a material with a higher density, such as a lead block. Since the code block has a larger density, the corresponding weight is greater under the same volume. When rotating around the mating shaft 9, the centrifugal force generated is greater; as the rotational speed of the mating shaft 9 increases, the rotational speed of the built-in stepped shaft 17 increases accordingly, thereby driving the counterweight 20 to rotate around the mating shaft 9. , causing the centrifugal force generated by the counterweight 20 to increase; the centrifugal force generated by the counterweight 20 drives the built-in stepped shaft 17 through the connecting rod 21 to have a downward tendency, thereby increasing the downward force of the pressure roller 18 and ultimately increasing the pressure roller 18 The breaking strength.
结合上述描述可知,本发明中压辊18与破碎筒8底部之间的挤压力包括了内置阶梯轴17所给予的下压力和压辊18的自重。 Based on the above description, it can be seen that the squeezing force between the pressure roller 18 and the bottom of the crushing cylinder 8 in the present invention includes the downward force given by the built-in stepped shaft 17 and the self-weight of the pressure roller 18 .
码块的材质根据实际生产需求可作出调整,例如铜块、铁块、铅块等;如此设置的目的在于,通过更换不同材质的码块,使得在相同转速下所产生的离心力不同,导致相同转速下压辊18施加的挤压力不同;可根据所需破碎的材料软硬程度适应性调整。The material of the code blocks can be adjusted according to actual production needs, such as copper blocks, iron blocks, lead blocks, etc.; the purpose of this setting is that by replacing the code blocks of different materials, the centrifugal force generated at the same speed will be different, resulting in the same The squeezing force exerted by the pressing roller 18 is different at the rotating speed; it can be adjusted adaptively according to the softness and hardness of the material to be crushed.
例如破碎硬度较大的物质时,可采用铅块;而对于硬度较小的物质时,可采用铁块或铜块。For example, when breaking materials with higher hardness, lead blocks can be used; while for materials with lower hardness, iron blocks or copper blocks can be used.
本发明中由于压辊18的破碎力主要由配重块20的离心力提供,因此该破碎力为柔性力,而非机械连接刚性力。In the present invention, since the crushing force of the pressure roller 18 is mainly provided by the centrifugal force of the counterweight 20, the crushing force is a flexible force rather than a rigid force of mechanical connection.
传统的破碎设备大多采用刚性力破碎,虽然能够达到破碎效率高的效果,但是同时也存在磨损严重的问题;而本发明中利用离心力提供破碎力,属于柔性力;若破碎筒8中存在个别变性的原料,导致其硬度相较于正常材料更高,无法通过一次滚压破碎时,本发明中的压辊18初次碾压该变性材料,可通过压辊18上抬让位的方式减小压辊18和破碎筒8底部的磨损;压辊18上抬过程中,通过转轴带动内置阶梯轴18在封闭腔16内向上滑动,进而利用连杆21带动配重块20靠近配合轴9;以达到避让效果;通过多次反复碾压该变性材料,使之慢慢被破碎,避免压辊18、转轴、以及破碎筒8底部超出其承压范围而产生变形或断裂。Most of the traditional crushing equipment uses rigid force for crushing. Although it can achieve high crushing efficiency, it also has the problem of serious wear. In the present invention, centrifugal force is used to provide crushing force, which is a flexible force; if there is individual degeneration in the crushing cylinder 8 When the hardness of the raw material is higher than that of normal materials and cannot be broken by one rolling, the pressure roller 18 in the present invention rolls the modified material for the first time, and the pressure can be reduced by lifting the pressure roller 18 to give way. The wear of the roller 18 and the bottom of the crushing drum 8; during the lifting process of the pressure roller 18, the built-in stepped shaft 18 is driven by the rotating shaft to slide upward in the closed cavity 16, and then the connecting rod 21 is used to drive the counterweight 20 close to the mating shaft 9; in order to achieve Avoidance effect: By repeatedly rolling the denatured material many times, it is slowly broken, preventing the pressure roller 18, the rotating shaft, and the bottom of the crushing drum 8 from exceeding their pressure-bearing range and causing deformation or breakage.
作为本发明再进一步的方案,顶盖2的顶部中央设置有法兰,并连接减速器;减速器通过传动结构与配合轴9连接;减速器一侧安装有马达4,马达4的转子轴连接减速器的输入端。通过马达4输出转矩,经减速器变速后向传动结构输出动力,最终由传动结构带动配合轴9旋转。As a further solution of the present invention, a flange is provided in the center of the top of the top cover 2 and is connected to a reducer; the reducer is connected to the mating shaft 9 through a transmission structure; a motor 4 is installed on one side of the reducer, and the rotor shaft of the motor 4 is connected The input end of the reducer. The motor 4 outputs torque, and then outputs power to the transmission structure after being changed by the speed reducer, and finally the transmission structure drives the matching shaft 9 to rotate.
作为本发明再进一步的方案,配合轴9的上部开设有贯通配合轴9顶部的上腔室15,上腔室15的内壁上开设有键槽14,键槽14平行于配合轴9的轴线;传动结构包括连接减速器输出端的传动轴6,传动轴6的下部外壁安装有卡键7,卡键7与键槽14适配。通过卡键7与键槽14配合实现传动轴6与配合轴9的连接,使得马达4输出的转矩通过减速器传递至传动轴6上,最终带动配合轴9旋转。As a further solution of the present invention, an upper chamber 15 that penetrates the top of the mating shaft 9 is provided on the upper part of the mating shaft 9. A keyway 14 is formed on the inner wall of the upper chamber 15. The keyway 14 is parallel to the axis of the mating shaft 9; the transmission structure It includes a transmission shaft 6 connected to the output end of the reducer, and a key 7 is installed on the lower outer wall of the transmission shaft 6, and the key 7 is adapted to the keyway 14. The transmission shaft 6 and the mating shaft 9 are connected through the cooperation of the key 7 and the keyway 14, so that the torque output by the motor 4 is transmitted to the transmission shaft 6 through the reducer, and finally drives the mating shaft 9 to rotate.
作为本发明再进一步的方案,顶盖2的边缘一体设置有吊耳,在预制罐1的外壁上安装有顶升机构3,顶升机构3具有一个动力缸体和一个伸出于动力缸体并与动力缸体伸缩配合的伸缩件;动力缸体与预制罐1固 定,伸缩件伸出动力缸体的一端与吊耳固定。通过顶升机构3中的动力缸体可带动伸缩件伸缩,进而带动吊耳和顶盖2升降,如此便可实现顶盖2与预制罐1顶口的分离和闭合;当顶盖2与预制罐1的顶口分离后,可向预制罐1内注入预混溶剂;同时还可向预制罐1内的破碎筒8中加入颗粒材料。As a further solution of the present invention, the edge of the top cover 2 is integrally provided with lifting lugs, and a lifting mechanism 3 is installed on the outer wall of the prefabricated tank 1. The lifting mechanism 3 has a power cylinder and a power cylinder extending from the power cylinder. telescopic parts that telescopically cooperate with the power cylinder block; the power cylinder block and the prefabricated tank 1 are fixed Fixed, one end of the telescopic part extends out of the power cylinder body and is fixed with the lifting eye. The power cylinder in the lifting mechanism 3 can drive the telescopic parts to expand and contract, thereby driving the lifting lugs and the top cover 2 to rise and fall, so that the top cover 2 can be separated and closed from the top of the prefabricated tank 1; when the top cover 2 and the top of the prefabricated tank 1 can be separated and closed; After the top opening of the prefabricated tank 1 is separated, the premixed solvent can be injected into the prefabricated tank 1; at the same time, granular materials can also be added to the crushing cylinder 8 in the prefabricated tank 1.
作为本发明再进一步的方案,均置分散组件包括转动设置在预制罐1内部中央的从动轴11,从动轴11顶部与配合轴9贯穿破碎筒8底部中央的一端同轴固定;从动轴11的底部悬空于预制罐1内并接近预制罐1的底部;从动轴11上沿圆周等距固定有多圈扭转叶片13。为了提高从动轴11的稳定性,在预制罐1内还固定有两组一号支架10,一号支架10的中心具有通孔;从动轴11穿过通孔并与之转动配合;在从动轴11上设置有两组凸缘,每组凸缘包含两圈凸起,同一组凸缘的两圈凸起分别位于两组一号支架10上的通孔两侧;利用通孔保持从动轴11始终位于预制罐1的中央,通过设置的凸缘使得从动轴11与通孔之间不会发生轴向错位。当配合轴9旋转时,可带动从动轴11跟随同步转动,进而驱使扭转叶片13转动,对预制罐1内的预混溶剂和干粉进行充分地分散,使得各成分的干粉均匀地溶置于预混溶剂中,加快各个材料之间的反应与融合。As a further solution of the present invention, the homogeneous dispersion assembly includes a driven shaft 11 that is rotated and arranged in the center of the interior of the prefabricated tank 1. The top of the driven shaft 11 and the matching shaft 9 are coaxially fixed with one end of the matching shaft 9 passing through the center of the bottom of the crushing drum 8; The bottom of the driving shaft 11 is suspended in the prefabricated tank 1 and is close to the bottom of the prefabricated tank 1; a plurality of twisting blades 13 are fixed on the driven shaft 11 at equal intervals along the circumference. In order to improve the stability of the driven shaft 11, two sets of No. 1 brackets 10 are fixed in the prefabricated tank 1. The center of the No. 1 bracket 10 has a through hole; the driven shaft 11 passes through the through hole and rotates with it; Two sets of flanges are provided on the driven shaft 11. Each set of flanges includes two rings of protrusions. The two rings of protrusions of the same set of flanges are respectively located on both sides of the through holes on the two sets of No. 1 brackets 10; using the through holes Keep the driven shaft 11 always located in the center of the prefabricated tank 1, and the flange provided prevents axial misalignment between the driven shaft 11 and the through hole. When the matching shaft 9 rotates, it can drive the driven shaft 11 to follow the synchronous rotation, thereby driving the twisting blade 13 to rotate, fully dispersing the premixed solvent and dry powder in the prefabricated tank 1, so that the dry powder of each component is evenly dissolved In premixed solvents, it accelerates the reaction and fusion between materials.
作为本发明再进一步的方案,预制罐1的底部安装有电磁阀5,电磁阀5与开设于预制罐1底部中央的排放口配合。当预制罐1内的各个成分的材料相互融合反应完全后,形成具有流动性的基材后,通过打开电磁阀5,可使预制罐1内的基材流出,流延排放于模具中。As a further solution of the present invention, a solenoid valve 5 is installed at the bottom of the prefabricated tank 1, and the solenoid valve 5 cooperates with the discharge port opened in the center of the bottom of the prefabricated tank 1. When the materials of each component in the prefabricated tank 1 are completely fused and reacted with each other to form a fluid base material, the solenoid valve 5 can be opened to allow the base material in the prefabricated tank 1 to flow out and be cast and discharged into the mold. .
本发明的设备在使用时的大致工作过程如下:The general working process of the equipment of the present invention when in use is as follows:
通过顶升机构3中的动力缸体带动伸缩件伸缩,进而带动吊耳和顶盖2升降,如此便可实现顶盖2与预制罐1顶口的分离和闭合;当顶盖2与预制罐1的顶口分离后,可向预制罐1内注入预混溶剂;同时还可向预制罐1内的破碎筒8中加入颗粒材料The power cylinder in the lifting mechanism 3 drives the telescopic parts to expand and contract, thereby driving the lifting lugs and the top cover 2 to rise and fall, so that the top cover 2 and the top opening of the prefabricated tank 1 can be separated and closed; when the top cover 2 and the prefabricated tank 1 are After the top opening of the can 1 is separated, the premixed solvent can be injected into the prefabricated tank 1; at the same time, granular materials can also be added to the crushing cylinder 8 in the prefabricated tank 1
而后反向启动动力缸体,可使顶盖2与预制罐1顶口闭合。Then the power cylinder is started in reverse, so that the top cover 2 and the top port of the prefabricated tank 1 can be closed.
启动马达4,通过马达4输出转矩并经减速器传递至传动轴6上,借助卡键7与键槽14配合实现传动轴6与配合轴9的连接,带动配合轴9旋转;配合轴9转动带动内置阶梯轴17跟随转动,从而带动压辊18在转 轴的作用下跟随内置阶梯轴17同步绕配合轴9旋转;随着配合轴9的转速增大,使得内置阶梯轴17的转速跟随增大,从而带动配重块20绕配合轴9旋转的转速增大,导致配重块20产生的离心力增大;配重块20产生的离心力通过连杆21带动内置阶梯轴17具有下压的趋势,从而使得压辊18的下压力增大,最终提高压辊18的破碎力度。Start the motor 4, and the torque output by the motor 4 is transmitted to the transmission shaft 6 through the reducer. The transmission shaft 6 and the mating shaft 9 are connected by the cooperation of the key 7 and the keyway 14, driving the mating shaft 9 to rotate; the mating shaft 9 rotates The built-in stepped shaft 17 is driven to follow the rotation, thereby driving the pressure roller 18 to rotate. Under the action of the shaft, the built-in stepped shaft 17 rotates synchronously around the mating shaft 9; as the rotational speed of the mating shaft 9 increases, the rotational speed of the built-in stepped shaft 17 increases accordingly, thereby driving the counterweight 20 to rotate around the mating shaft 9. increases, causing the centrifugal force generated by the counterweight 20 to increase; the centrifugal force generated by the counterweight 20 drives the built-in stepped shaft 17 through the connecting rod 21 to have a downward pressure, thereby increasing the downward force of the pressure roller 18 and ultimately increasing the pressure. The crushing strength of roller 18.
而传统的研磨设备在电机启动后便会对物料进行破碎,尤其时在电机尚未达到额定转速时,由于压碾的力度不能够匹配电机转速,导致电机启动之初的负载较大,极易烧毁电机。Traditional grinding equipment will crush the materials after the motor is started. Especially when the motor has not reached the rated speed, the crushing force cannot match the motor speed, resulting in a large load at the beginning of the motor start-up and it is easy to burn out. motor.
此外,传统的破碎设备大多采用刚性力破碎,虽然能够达到破碎效率高的效果,但是同时也存在磨损严重的问题;而本发明中利用离心力提供破碎力,属于柔性力;若破碎筒8中存在个别变性的原料,导致其硬度相较于正常材料更高,无法通过一次滚压破碎时,本发明中的压辊18初次碾压该变性材料,可通过压辊18上抬让位的方式减小压辊18和破碎筒8底部的磨损;压辊18上抬过程中,通过转轴带动内置阶梯轴18在封闭腔16内向上滑动,进而利用连杆21带动配重块20靠近配合轴9;以达到避让效果;通过多次反复碾压该变性材料,使之慢慢被破碎,避免压辊18、转轴、以及破碎筒8底部超出其承压范围而产生变形或断裂。In addition, most traditional crushing equipment uses rigid force for crushing. Although it can achieve high crushing efficiency, it also has the problem of serious wear. In the present invention, centrifugal force is used to provide crushing force, which is a flexible force; if there is When some denatured raw materials have a higher hardness than normal materials and cannot be broken by one rolling, the pressure roller 18 in the present invention can crush the denatured material for the first time, and the pressure roller 18 can be lifted up to give way. Wear of the small pressure roller 18 and the bottom of the crushing drum 8; during the lifting process of the pressure roller 18, the built-in stepped shaft 18 is driven by the rotating shaft to slide upward in the closed cavity 16, and then the connecting rod 21 is used to drive the counterweight 20 close to the mating shaft 9; In order to achieve the avoidance effect; by repeatedly rolling the denatured material many times, it is slowly crushed to prevent the pressure roller 18, the rotating shaft, and the bottom of the crushing drum 8 from exceeding their pressure-bearing range and causing deformation or breakage.
当配合轴9旋转时,可带动从动轴11跟随同步转动,进而驱使扭转叶片13转动,对预制罐1内的预混溶剂和干粉进行充分地分散,使得各成分的干粉均匀地溶置于预混溶剂中,加快各个材料之间的反应与融合。When the matching shaft 9 rotates, it can drive the driven shaft 11 to follow the synchronous rotation, thereby driving the twisting blade 13 to rotate, fully dispersing the premixed solvent and dry powder in the prefabricated tank 1, so that the dry powder of each component is evenly dissolved In premixed solvents, it accelerates the reaction and fusion between materials.
在配合轴9的转速增大的过程中,与配合轴9机械连接的从动轴11转速也随之增大,使得不断增加并投入到预制罐1内的干粉能够及时有效地与预混溶剂混合反应。In the process of increasing the rotation speed of the matching shaft 9, the rotation speed of the driven shaft 11 that is mechanically connected to the matching shaft 9 also increases, so that the dry powder that is continuously increased and put into the prefabricated tank 1 can be mixed with the preform in a timely and effective manner. Solvent mixing reaction.
本发明应用了具体个例对本发明的原理及实施方式进行了阐述,以上实施例的说明只是用于帮助理解本发明的方法及其核心思想;同时,对于本领域的一般技术人员,依据本发明的思想,在具体实施方式及应用范围上均会有改变之处。综上,本说明书内容不应理解为对本发明的限制。 The present invention uses specific examples to illustrate the principles and implementation methods of the present invention. The description of the above embodiments is only used to help understand the method of the present invention and its core idea; at the same time, for those of ordinary skill in the art, according to the present invention There will be changes in the specific implementation methods and application scope of the ideas. In summary, the contents of this description should not be construed as limitations of the present invention.

Claims (7)

  1. 一种氮化硅吸波材料的生产设备,用于在氮化硅吸波材料的生产工艺中,配制预混溶剂、预备干粉、以及制备基材;其特征在于,包括预制罐(1)和活动设置在所述预制罐(1)顶口上方的顶盖(2);所述顶盖(2)可将预制罐(1)的顶口封闭;当顶盖(2)严密贴合预制罐(1)的顶口时,预制罐(1)和顶盖(2)之间形成一个密封容器;A production equipment for silicon nitride absorbing materials, used to prepare premixed solvents, prepare dry powder, and prepare base materials in the production process of silicon nitride absorbing materials; it is characterized by including a prefabricated tank (1) and a top cover (2) movably arranged above the top of the prefabricated tank (1); the top cover (2) can seal the top of the prefabricated tank (1); when the top cover (2) is tightly attached When the top of the prefabricated tank (1) is closed, a sealed container is formed between the prefabricated tank (1) and the top cover (2);
    还包括:Also includes:
    制粉组件,所述制粉组件包括通过一号支架(10)固定在所述预制罐(1)内部上层中央的破碎筒(8),以及设置在所述破碎筒(8)内的碾压结构;当所述碾压结构绕所述破碎筒(8)的中心轴线转动时,可沿圆周对破碎筒(8)内的颗粒物进行压碾;且压碾力度同碾压结构的转速呈正相关关系;Powder making assembly, the powder making assembly includes a crushing drum (8) fixed at the center of the upper layer inside the prefabricated tank (1) through the No. 1 bracket (10), and a grinding mill installed in the crushing drum (8). The crushing structure; when the crushing structure rotates around the central axis of the crushing barrel (8), the particles in the crushing barrel (8) can be crushed along the circumference; and the crushing force is positive to the rotation speed of the crushing structure. relationship;
    均置分散组件,所述均置分散组件设置于所述预制罐(1)内,并与所述碾压结构机械配合,以使压碾成粉并掉落至预制罐(1)内的干粉能够与预制罐(1)内的预混溶剂充分接触,混合反应;A homogeneous dispersion component is arranged in the prefabricated tank (1) and mechanically cooperates with the rolling structure to crush it into powder and fall into the prefabricated tank (1). The dry powder can fully contact with the premixed solvent in the preformed tank (1) for mixing and reaction;
    所述碾压结构包括贯穿所述破碎筒(8)底部中央并与之密封转动连接的配合轴(9)、等距分布在所述配合轴(9)外周的多个压辊(18)、以及设置在所述配合轴(9)上并连接所述压辊(18)的调压机构;The rolling structure includes a matching shaft (9) that penetrates the center of the bottom of the crushing drum (8) and is sealed and rotationally connected with it, a plurality of pressure rollers (18) equidistantly distributed around the outer circumference of the matching shaft (9), And a pressure regulating mechanism provided on the matching shaft (9) and connected to the pressure roller (18);
    当所述配合轴(9)旋转时可带动多个压辊(18)在破碎筒(8)内绕配合轴(9)旋转;且压辊(18)与破碎筒(8)底部贴合,对破碎筒(8)内的颗粒材料破碎;When the matching shaft (9) rotates, it can drive multiple pressure rollers (18) to rotate around the matching shaft (9) in the crushing barrel (8); and the pressure rollers (18) fit with the bottom of the crushing barrel (8), Crushing the granular materials in the crushing cylinder (8);
    在所述破碎筒(8)的底部均匀开设有多个滤孔;A plurality of filter holes are evenly provided at the bottom of the crushing drum (8);
    所述配合轴(9)的内部中央设置有封闭腔(16),封闭腔(16)内活动设 置有内置阶梯轴(17);所述内置阶梯轴(17)与所述配合轴(9)同轴,且其可在封闭腔(16)内沿其轴线活动;A closed cavity (16) is provided in the center of the matching shaft (9), and a movable device is provided in the closed cavity (16). There is a built-in stepped shaft (17); the built-in stepped shaft (17) is coaxial with the matching shaft (9), and it can move along its axis in the closed cavity (16);
    所述压辊(18)通过转轴与内置阶梯轴(17)转动连接,在所述配合轴(9)上开设有连通所述封闭腔(16)的第二穿槽(24),所述转轴穿过第二穿槽(24)与封闭腔(16)内的内置阶梯轴(17)转动连接;The pressure roller (18) is rotatably connected to the built-in stepped shaft (17) through a rotating shaft, and a second through groove (24) connected to the closed cavity (16) is provided on the matching shaft (9). The rotating shaft It passes through the second through groove (24) and is rotatably connected to the built-in stepped shaft (17) in the closed cavity (16);
    所述第二穿槽(24)平行于所述配合轴(9)的轴线开设,调压机构连接所述内置阶梯轴(17);The second through groove (24) is opened parallel to the axis of the matching shaft (9), and the pressure regulating mechanism is connected to the built-in stepped shaft (17);
    所述调压机构包括沿圆周固定在所述配合轴(9)外壁上的托板(19)、滑动设置在所述托板(19)上的配重块(20)、以及连接所述配重块(20)与所述内置阶梯轴(17)的连杆(21);The pressure regulating mechanism includes a supporting plate (19) circumferentially fixed on the outer wall of the mating shaft (9), a counterweight (20) slidably disposed on the supporting plate (19), and a counterweight connected to the supporting plate (19). The connecting rod (21) between the weight (20) and the built-in stepped shaft (17);
    在所述配合轴(9)上开设有连通所述封闭腔(16)上部的第一穿槽(23);连杆(21)的一端与所述配重块(20)铰接,另一端与内置阶梯轴(17)的外壁铰接;A first through groove (23) connected to the upper part of the closed cavity (16) is provided on the matching shaft (9); one end of the connecting rod (21) is hinged with the counterweight (20), and the other end is connected with the counterweight (20). The outer wall of the built-in stepped shaft (17) is hinged;
    所述托板(19)沿所述配合轴(9)的径向设置,配重块(20)沿所述配合轴(9)的径向滑动设置在所述托板(19)上。The supporting plate (19) is arranged along the radial direction of the fitting shaft (9), and the counterweight (20) is slidably arranged on the supporting plate (19) along the radial direction of the fitting shaft (9).
  2. 根据权利要求1所述的一种氮化硅吸波材料的生产设备,其特征在于,所述均置分散组件包括转动设置在所述预制罐(1)内部中央的从动轴(11),所述从动轴(11)顶部与配合轴(9)贯穿破碎筒(8)底部中央的一端同轴固定;A silicon nitride absorbing material production equipment according to claim 1, characterized in that the uniform dispersion assembly includes a driven shaft (11) that is rotationally arranged in the center of the interior of the prefabricated tank (1). , the top of the driven shaft (11) and the end of the matching shaft (9) penetrating through the center of the bottom of the crushing barrel (8) are coaxially fixed;
    从动轴(11)的底部悬空于所述预制罐(1)内并接近预制罐(1)的底部;从动轴(11)上沿圆周等距固定有多圈扭转叶片(13)。The bottom of the driven shaft (11) is suspended in the prefabricated tank (1) and is close to the bottom of the prefabricated tank (1); multiple turns of torsion blades (13) are fixed equidistantly along the circumference of the driven shaft (11). .
  3. 根据权利要求1所述的一种氮化硅吸波材料的生产设备,其特征在 于,所述顶盖(2)的顶部中央设置有法兰,并连接减速器;所述减速器通过传动结构与所述配合轴(9)连接;所述减速器一侧安装有马达(4),所述马达(4)的转子轴连接减速器的输入端。A silicon nitride absorbing material production equipment according to claim 1, characterized in that Therefore, a flange is provided in the center of the top of the top cover (2) and is connected to a reducer; the reducer is connected to the matching shaft (9) through a transmission structure; a motor (4) is installed on one side of the reducer ), the rotor shaft of the motor (4) is connected to the input end of the reducer.
  4. 根据权利要求3所述的一种氮化硅吸波材料的生产设备,其特征在于,所述配合轴(9)的上部开设有贯通所述配合轴(9)顶部的上腔室(15),所述上腔室(15)的内壁上开设有键槽(14),键槽(14)平行于所述配合轴(9)的轴线;The production equipment of silicon nitride absorbing material according to claim 3, characterized in that an upper chamber (15) penetrating the top of the matching shaft (9) is provided on the upper part of the matching shaft (9). , a keyway (14) is provided on the inner wall of the upper chamber (15), and the keyway (14) is parallel to the axis of the matching shaft (9);
    所述传动结构包括连接所述减速器输出端的传动轴(6),所述传动轴(6)的下部外壁安装有卡键(7),所述卡键(7)与所述键槽(14)适配。The transmission structure includes a transmission shaft (6) connected to the output end of the reducer. A key (7) is installed on the lower outer wall of the transmission shaft (6). The key (7) and the keyway (14) adaptation.
  5. 根据权利要求1所述的一种氮化硅吸波材料的生产设备,其特征在于,所述顶盖(2)的边缘一体设置有吊耳,在预制罐(1)的外壁上安装有顶升机构(3),所述顶升机构(3)具有一个动力缸体和一个伸出于所述动力缸体并与动力缸体伸缩配合的伸缩件;The production equipment of silicon nitride absorbing material according to claim 1, characterized in that the edge of the top cover (2) is integrally provided with lifting lugs, and the outer wall of the prefabricated tank (1) is equipped with lifting lugs. Jacking mechanism (3), the jacking mechanism (3) has a power cylinder and a telescopic member that extends from the power cylinder and telescopically cooperates with the power cylinder;
    所述动力缸体与预制罐(1)固定,伸缩件伸出所述动力缸体的一端与吊耳固定。The power cylinder is fixed to the prefabricated tank (1), and one end of the telescopic component extending out of the power cylinder is fixed to the lifting eye.
  6. 根据权利要求1所述的一种氮化硅吸波材料的生产设备,其特征在于,所述预制罐(1)的底部安装有电磁阀(5),所述电磁阀(5)与开设于所述预制罐(1)底部中央的排放口配合。A silicon nitride absorbing material production equipment according to claim 1, characterized in that a solenoid valve (5) is installed at the bottom of the prefabricated tank (1), and the solenoid valve (5) is connected to an opening. Match it with the discharge port in the center of the bottom of the prefabricated tank (1).
  7. 一种使用如权利要求1-5任一项所述的设备生产氮化硅吸波材料的工艺,其特征在于,包括如下步骤:A process for producing silicon nitride absorbing materials using the equipment according to any one of claims 1 to 5, characterized in that it includes the following steps:
    步骤一,配制预混溶剂,将丙烯酰胺和交联剂溶于乙醇中制备预混溶剂,并用氨水调剂溶剂的pH; Step 1: Prepare a premixed solvent, dissolve acrylamide and cross-linking agent in ethanol to prepare the premixed solvent, and adjust the pH of the solvent with ammonia water;
    步骤二,预备干粉,对氮化硅基体、氯化铁颗粒、聚甲基丙烯酸甲酯颗粒、碳基纤维、以及氧化铝颗粒破碎,制成粉末混合备用;Step 2: Prepare dry powder, crush the silicon nitride matrix, ferric chloride particles, polymethylmethacrylate particles, carbon-based fibers, and alumina particles to make a powder and mix it for later use;
    步骤三,基材制备,将粉状的氮化硅基体、氯化铁、聚甲基丙烯酸甲酯、碳基纤维、以及氧化铝同预混溶剂混合,各组分相互融合反应,生成胶状基材;Step 3: Prepare the substrate. Mix the powdered silicon nitride matrix, ferric chloride, polymethylmethacrylate, carbon-based fiber, and alumina with the premixed solvent. The components will fuse and react with each other to form a gel. base material;
    步骤四,材料成型,将制备的基材排入到模具中流延成型,合模后抽真空,于常温下干燥;干燥8~15小时后脱模形成坯材,并对坯材干压脱胶;Step 4: Material molding. Put the prepared base material into the mold for tape casting. After closing the mold, vacuum and dry at room temperature. After drying for 8 to 15 hours, the mold is demoulded to form a blank, and the blank is dry-pressed and degummed;
    步骤五,烧结,将脱胶后的坯材置于氮气氛围下反应烧结 Step five, sintering, place the degummed blank in a nitrogen atmosphere for reaction sintering.
PCT/CN2023/103526 2022-09-05 2023-06-29 Production process and device for silicon nitride wave-absorbing material WO2024051305A1 (en)

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