GB2625431A - Silicon nitride wave-transmitting material, preparation process and preparation apparatus - Google Patents
Silicon nitride wave-transmitting material, preparation process and preparation apparatus Download PDFInfo
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- GB2625431A GB2625431A GB2316471.8A GB202316471A GB2625431A GB 2625431 A GB2625431 A GB 2625431A GB 202316471 A GB202316471 A GB 202316471A GB 2625431 A GB2625431 A GB 2625431A
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 70
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 52
- 239000000463 material Substances 0.000 title claims abstract description 33
- 239000002002 slurry Substances 0.000 claims abstract description 99
- 238000002156 mixing Methods 0.000 claims abstract description 58
- 239000012780 transparent material Substances 0.000 claims abstract description 42
- 239000000843 powder Substances 0.000 claims abstract description 38
- 239000002994 raw material Substances 0.000 claims abstract description 29
- 238000007670 refining Methods 0.000 claims abstract description 17
- 238000007789 sealing Methods 0.000 claims abstract description 16
- 230000007246 mechanism Effects 0.000 claims abstract description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 90
- 238000000227 grinding Methods 0.000 claims description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- 239000011148 porous material Substances 0.000 claims description 38
- 239000003795 chemical substances by application Substances 0.000 claims description 28
- 230000005540 biological transmission Effects 0.000 claims description 27
- 239000002270 dispersing agent Substances 0.000 claims description 27
- 239000002245 particle Substances 0.000 claims description 27
- 239000003431 cross linking reagent Substances 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 10
- 238000005086 pumping Methods 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 238000005096 rolling process Methods 0.000 claims description 4
- 238000005452 bending Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 16
- 230000008569 process Effects 0.000 abstract description 13
- 238000012546 transfer Methods 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 5
- 238000010298 pulverizing process Methods 0.000 abstract 3
- 239000011344 liquid material Substances 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 238000010586 diagram Methods 0.000 description 9
- 229910052786 argon Inorganic materials 0.000 description 5
- 229910052754 neon Inorganic materials 0.000 description 5
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000012826 global research Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/10—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by using foaming agents or by using mechanical means, e.g. adding preformed foam
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- 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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- 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
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
- C04B2235/3873—Silicon nitrides, e.g. silicon carbonitride, silicon oxynitride
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Abstract
A silicon nitride wave-transparent material preparation apparatus, comprising a slurry tank (1); a sealing cover (2) arranged on the upper part of the slurry tank; a pulverizing cylinder (3) arranged above the slurry tank and communicated with the interior of the slurry tank by means of a through hole formed in the center of the sealing cover; a refining mechanism arranged in the pulverizing cylinder; and a blending assembly arranged in the slurry tank. Solid raw materials are refined in the pulverizing cylinder, and then can be directly put into the slurry tank containing liquid materials without intermediate transfer, preventing the refined powder material from being doped with other substances in the intermediate transfer process; in addition, the intermediate transfer procedure is eliminated, so that the preparation period is shortened.
Description
SILICON NITRIDE WAVE-TRANSPARENT MATERIAL, AND PREPARATION
PROCESS AND PREPARATION DEVICE THEREOF
TECHNICAL FIELD
[0001] The present disclosure relates to a technology related to chemical materials, and specifically provides a silicon nitride wave-transparent material, and a preparation process and a preparation device thereof
BACKGROUND
[0002] Wave-transparent materials generally have high electromagnetic wave transmittance and low dielectric constant and loss, and are widely used in launch vehicles, spacecrafts, missiles, and returnable satellites. In recent years, nitride ceramic materials have become one of the hot topics of global research due to excellent properties.
[0003] Si3N4 ceramic shows desirable mechanical properties at both high and normal temperatures, as well as satisfactory thermal stability, low dielectric loss, and high erosion resistance, and is a wave-transparent material with excellent comprehensive properties. The production of silicon nitride wave-transparent materials is basically inseparable from the processes of ball milling, mixing, molding, and sintering.
[0004] Currently, when industrially producing a silicon nitride wave-transparent material, silicon nitride, aluminium oxide, a pore-forming agent, and a dispersant in raw materials require to be finely crushed, and then obtained finely crushed raw materials are dissolved in a solvent. During this process, fine crushing and dissolving are completed in two procedures. When the two procedures are connected (including discharging and loading), exposure is inevitable, which increases the risk of impurities being mixed This affects the stable development of crystal phases due to impurities during the preparation of the silicon nitride wave-transparent material.
SUMMARY
[0005] An objective of the present disclosure is to provide a silicon nitride wave-transparent material, and a preparation process and a preparation device thereof, so as to solve the problems raised in the background.
[0006] To achieve the above objective, the present disclosure provides the following technical solutions: [0007] The present disclosure provides a silicon nitride wave-transparent material, including the following raw materials: 35 parts of a cross-linking agent, 30 parts of industrial ethanol, 25 parts of silicon nitride particles, 5 parts of aluminium oxide powder, 3 parts of a pore-forming agent, and 2 parts of a dispersant.
100081 The present disclosure further provides a preparation process of the silicon nitride wave-transparent material, including the following steps: sl, production of a powder raw material of slurry. refining the silicon nitride particles, the aluminium oxide powder, the pore-forming agent, and the dispersant; s2, blending and preparation of the slurry: putting the refined powder raw material of the slurry into a container containing deionized water and the industrial ethanol to allow mixing; dispersing the silicon nitride, the aluminium oxide, and the pore-forming agent evenly into a solvent obtained by mixing the cross-linking agent and the industrial ethanol under an action of the dispersant; and introducing a protective gas into the container while mixing; s3, slurry discharging and forming: transferring the prepared slurry from the container into a mold to form a layered structure, and controlling a thickness of each layer to form a prefabricated material blank; and s4, sintering and molding: stacking the prefabricated material blank with different layered structures according to predetermined layer levels, and conducting sintering in a nitrogen environment at a pressure of 1 MPa to 1.5 MPa and at a temperature of 1,500C to 1,9501C for 2 h to 5 h. 100091 The present disclosure further provides a preparation device of a silicon nitride wave-transparent material, where the preparation device is configured to produce a powder raw material of slurry, and mix a liquid raw material with the powder raw material to obtain the slurry in a preparation process of the silicon nitride wave-transparent material; wherein the preparation device comprises: a slurry tank, a sealing cover is arranged on an upper part of the slurry tank, a perforation is arranged in a center of the sealing cover, wherein a powder-making cylinder is arranged on the perforation in a sealed manner, and the powder-making cylinder communicates with an interior of the slurry tank through the perforation; wherein a refining mechanism is provided in the powder-making cylinder, the refining mechanism is configured to refine silicon nitride particles, aluminium oxide powder, a pore-forming agent, and a dispersant; and wherein a blending component is provided in the slurry tank, the blending component is configured to uniformly disperse the silicon nitride particles, the aluminium oxide powder, the pore-forming agent, and the dispersant that are refined into a solvent obtained by mixing a cross-linking agent and industrial ethanol.
[0010] In the preparation device of a silicon nitride wave-transparent material, the refining mechanism includes: a primary crushing cylinder fixedly arranged in the powder-making cylinder, wherein a plurality of primary sieve pores are evenly arranged in a lower part of the primary crushing cylinder; a grinding head movably arranged in the primary crushing cylinder; the grinding head is movable up and down in the primary crushing cylinder to grind the silicon nitride particles, the aluminium oxide powder, the pore-forming agent, and the dispersant in conjunction with a lower inner wall of the primary crushing cylinder; and a gap is formed between an outer periphery of the grinding head and the lower inner wall of the primary crushing cylinder, so as to allow an original material poured from an upper port of the powder-making cylinder to enter the primary crushing cylinder; a secondary crushing cylinder rotatably arranged outside the primary crushing cylinder, wherein a plurality of secondary sieve pores are evenly arranged in a lower part of the secondary crushing cylinder, and the secondary crushing cylinder and the primary crushing cylinder are in a same shape; wherein a gap is formed between a lower inner wall of the secondary crushing cylinder and a lower outer wall of the primary crushing cylinder; the secondary sieve pores have a pore size smaller than a pore size of the primary sieve pores, and the gap between the lower inner wall of the secondary crushing cylinder and the lower outer wall of the primary crushing cylinder is smaller than the pore size of the primary sieve pores; and wherein when the grinding head moves up and down in the primary crushing cylinder, the secondary crushing cylinder rotates around the primary crushing cylinder.
100111 In the preparation device of a silicon nitride wave-transparent material, a frame structure is fixedly arranged on the sealing cover, a crankshaft is horizontally and rotatably arranged on the frame structure, a bending portion at a middle of the crankshaft is rotatably sleeved with an upper end of a connecting rod, and a lower end of the connecting rod is rotatably fitted with an upper part of a driving rod through a pin.
[0012] The grinding head is fixed on a lower end of the driving rod, a support is fixed inside the powder-making cylinder, a grinding sleeve is fixed in a center of the support, and the driving rod penetrates the grinding sleeve and is slidably fitted with the grinding sleeve [0013] In the preparation device of a silicon nitride wave-transparent material, a transmission rod is further provided between the frame structure and the powder-making cylinder, and the transmission rod is arranged vertically, wherein a lower end and a central portion of the transmission rod are rotatably fitted with an outer wall of the powder-making cylinder; an upper shaft journal of the transmission rod is rotatably fitted with a bracket fixed on an inner side of the frame structure.
[0014] An upper end of the transmission rod is connected to the crankshaft through a bevel gear set, and a rotating gear is fixed at a lower part of the transmission rod; a ring gear is fixed on an outer wall of the secondary crushing cylinder, a notch is arranged at a side of the powder-making cylinder close to the rotating gear, and the rotating gear crosses the notch and meshes with the ring gear.
100151 In the preparation device of a silicon nitride wave-transparent material, the mixing shaft is rotatably arranged in the slurry tank, and both ends of the mixing shaft penetrate the slurry tank and are rotatably fitted with the slurry tank in a sealed manner.
[0016] One end of the mixing shaft is connected to an output end of a mixing motor fixedly arranged on an outer wall of the slurry tank, and the mixing shaft is provided with a plurality of sets of blades.
[0017] A lower part of the slurry tank is in a shape of an inverted pagoda, and a gate valve is arranged at a bottom of the slurry tank.
[0018] In the preparation device of a silicon nitride wave-transparent material, the air pump is fixedly arranged on the outer wall of the slurry tank, an impeller shaft of the air pump is coaxially fixed with a pumping shaft, and the pumping shaft is connected to an other one end of the mixing shaft through a transmission belt [0019] An air outlet end of the air pump penetrates the outer wall of the slurry tank, an air box is fixed on an inner wall of the slurry tank, and an air chamber is fon-ned between the air box and the inner wall of the slurry tank 100201 The air outlet end of the air pump is connected to the air chamber, a plurality of manifolds are connected to the air chamber, and the manifolds are close to the inner wall of the slurry tank and extends to the bottom of the slurry tank.
[0021] In the preparation device of a silicon nitride wave-transparent material, a circle of track is arranged on a lower inner wall of the powder-making cylinder, a plurality of carrier rollers are arranged in a circumference at equal intervals on an outer periphery of the secondary crushing cylinder, the carrier rollers are rotatably arranged on the outer wall of the secondary crushing cylinder, and the carrier rollers are fitted in the track in a rolling manner.
[0022] In the preparation device of a silicon nitride wave-transparent material, an upper inner wall of the powder-making cylinder is provided with a circle of recess, an upper outer wall of the primary crushing cylinder is provided with a circle of protrusion, and the protrusion is fitted inside the recess.
[0023] The primary crushing cylinder is provided with a plurality of screw holes, the plurality of screw holes are equidistantly distributed along an outer periphery of the primary crushing cylinder, and the screw holes penetrate the recess; and a plurality of counter bores corresponding to the screw holes are arranged on the protrusion.
[0024] The powder-making cylinder and the primary crushing cylinder are fixed by bolts, and the bolts match threads of the screw holes and extend into the counter bores.
[0025] Compared with the existing technology, some embodiments has the following beneficial effects: by arranging the refining mechanism in the powder-making cylinder, the silicon nitride particles, the aluminium oxide powder, the pore-forming agent, and the dispersant can be directly put into the slurry tank containing the cross-linking agent and industrial ethanol after being refined. The preparation device does not require intermediate transfer so as to avoid the doping of other substances during the intermediate transfer of the refined silicon nitride particles, aluminium oxide powder, pore-forming agent, and dispersant.
[0026] In addition, the process of the intermediate transfer is reduced, the preparation process of the silicon nitride wave-transparent material is simplified, and a preparation cycle is shortened.
BRIEF DESCRIPTION OF THE DRAWINGS
[0027] FIG. 1 shows a schematic structural diagram of the preparation device of a silicon nitride wave-transparent material; [0028] FIG. 2 shows another schematic structural diagram of the preparation device of a silicon nitride wave-transparent material; [0029] FIG. 3 shows a schematic diagram of the refining mechanism and the frame structure in the preparation device of a silicon nitride wave-transparent material; 100301 FIG. 4 shows s schematic structural diagram of FIG. 3 after offset; 100311 FIG. 5 shows a schematic structural diagram of the refining mechanism after disassembly; 100321 FIG. 6 shows a schematic structural diagram of the powder-making cylinder after a partial section; [0033] FIG. 7 shows a schematic structural diagram of the blending component in the preparation device of a silicon nitride wave-transparent material; [0034] FIG. 8 shows a schematic structural diagram of FIG. 7 after the slurry tank is removed; and [0035] FIG. 9 shows s schematic structural diagram of FIG. 7 after offset.
[0036] List of reference numerals: 1-slurry tank; 2-sealing cover; 3-powder-making cylinder; 4-frame structure; 5-crankshaft; 6-gear motor; 7-connecting rod; 8-driving rod; 9-grinding head; 10-grinding sleeve; 11-primary crushing cylinder; 12-secondary crushing cylinder; 13-protrusion; 14-carrier roller; 15-recess; 16-track; 17-driving gear; 18-driven gear; 19-transmission rod; 20-rotating gear; 21-notch; 22-ring gear; 23-mixing motor; 24-mixing shaft; 25-blade; 26-transmission belt; 27-pumping shaft; 28-air pump; 29-manifold; 30-gate valve.
DETAILED DESCRIPTION OF THE EMBODIMENTS
100371 The technical solutions in the embodiments of the present disclosure will be described clearly and completely hereinafter with reference to the drawings of the embodiments of the present disclosure. Apparently, the described embodiments are some embodiments of the present disclosure, rather than all of the embodiments.
[0038] As an example of the present disclosure, a silicon nitride wave-transparent material included the following raw materials: 35 g of a cross-linking agent, 30 g of industrial ethanol, 25 g of silicon nitride particles, 5 g of aluminium oxide powder, 3 g of a pore-forming agent, and 2 g of a dispersant.
[0039] The aluminium oxide powder and the pore-forming agent are added to the silicon nitride particles, such that crystals of the material can be directionally developed to form honeycomb holes, which increases a pore structure of the material presented in this embodiment and the material endows an excellent wave transmission performance; meanwhile, the aluminium oxide powder increases the rates of dissolution and precipitation of silicon nitride during the crystal phase change in a high-temperature environment. The crystal phase change does not increase the density of the material, thereby further improving the wave-transparent performance.
100401 In addition, the aluminium oxide powder combined with the industrial ethanol and the cross-linking agent can control a dielectric constant of the material in this embodiment and reduce the dielectric loss; this measure can also reduce the liquid phase and increase the viscosity.
100411 The interconnected pore structures form an angular interaction with each other, which improved the mechanical strength of the material in this embodiment and also achieved a lightweight design of the material; on the basis of saving materials, the output of products is increased.
[0042] This embodiment further provides a preparation process of the silicon nitride wave-transparent material, including the following steps: sl, production of a powder raw material of slurry: the silicon nitride particles, the aluminium oxide powder, the pore-forming agent, and the dispersant are refined, where the slurry has a particle size controlled at 70 pm to 120 pm; s2, blending and preparation of the slurry: a the refined slurry powder is put into a container containing deionized water and the industrial ethanol to allow mixing; dispersing the silicon nitride, the aluminium oxide, and the pore-forming agent evenly into a solvent obtained by mixing the cross-linking agent and the industrial ethanol under an action of the dispersant, such that dielectric properties of the slurry are controlled with industrial ethanol; and a protective gas, such as argon or neon, is introduced into the container to ensure a stability of the material properties of the slurry; s3, slurry discharging and forming: a prepared slurry is transferred from the container into a mold to form a layered structure, and a thickness of each layer is controlled to form a prefabricated material blank; and s4, sintering and molding: the prefabricated material blank with different layered structures is stacked according to predetermined layer levels, and sintering is conducted in a nitrogen environment at a pressure of 1 MPa to 1.5 MPa and at a temperature of 1,500 t to 1,950°C for 2 h to 5 h. 100431 In the process of this embodiment, the wave-transparent material stacked in multiple layer levels can adapt to wide-band operating conditions, and a composite structure can be formed by controlling the cooperation between each layer level. Therefore, performance, adjustment and control are optimized.
[0044] This embodiment further provided a preparation device used for the preparation process of a silicon nitride wave-transparent material. This device is mainly used for the production of a powder raw material of the slurry and blending and preparation of the slurry in the preparation process of a silicon nitride wave-transparent material. Referring to FIG. 1 to FIG. 2, the device included: a slurry tank 1, a sealing cover 2 is arranged on an upper part of the slurry tank 1, a perforation is arranged in a center of the sealing cover 2, where a powder-making cylinder 3 is arranged on the perforation in a sealed manner, and the powder-making cylinder 3 communicates with an interior of the slurry tank 1 through the perforation; wherein a refining mechanism is provided in the powder-making cylinder 3 and the refining mechanism is configured to refine a silicon nitride particles, aluminium oxide powder, a pore-forming agent, and a dispersant; and wherein a blending component is provided in the slurry tank 1, the blending component is configured to uniformly disperse the silicon nitride particles, the aluminium oxide powder, the pore-forming agent, and the dispersant that are refined into a solvent obtained by mixing the cross-linking agent and the industrial ethanol.
100451 Specifically, a lower edge of the powder-making cylinder 3 is in sealing fit with an upper surface of the sealing cover 2 and is tightly fixed by bolts; a plurality of reinforcing ribs are further provided on the sealing cover 2, and a plurality of the reinforcing ribs are connected with each other to form a closed structure, so as to improve a bearing capacity of the sealing cover 2 to the powder-making cylinder 3 100461 In this embodiment, by arranging the refining mechanism in the powder-making cylinder 3, the silicon nitride particles, the aluminium oxide powder, the pore-forming agent, and the dispersant can be directly put into the slurry tank 1 containing the cross-linking agent and the industrial ethanol after being refined. The intermediate transfer is not required so as to avoid the doping of other substances during the intermediate transfer of the refined silicon nitride particles, aluminium oxide powder, pore-forming agent, and dispersant.
100471 In addition, the process of the intermediate transfer is reduced, the preparation process of the silicon nitride wave-transparent material is simplified, and a preparation cycle is shortened. 100481 As a further solution of this example, referring to FIG. 1 to FIG. 6, the refining mechanism included.
a primary crushing cylinder 11, wherein the primary crushing cylinder 11 is fixedly arranged in the powder-making cylinder 3, and a plurality of primary sieve pores are evenly arranged in a lower part of the primary crushing cylinder 11; a grinding head 9, wherein the grinding head 9 is movably arranged in the primary crushing cylinder 11; the grinding head 9 is movable up and down in the primary crushing cylinder 11 to grind the silicon nitride particles, the aluminium oxide powder, the pore-forming agent, and the dispersant in conjunction with a lower inner wall of the primary crushing cylinder 11, and a gap is formed between an outer periphery of the grinding head 9 and the lower inner wall of the primary crushing cylinder 11, so as to allow an original material poured from an upper port of the powder-making cylinder 3 to enter the primary crushing cylinder 11 and be positioned between the grinding head 9 and the lower inner wall of the primary crushing cylinder 11; a secondary crushing cylinder 12, wherein the secondary crushing cylinder 12 is rotatably arranged outside the primary crushing cylinder 11, a plurality of secondary sieve pores are evenly arranged in a lower part of the secondary crushing cylinder 12, and the secondary crushing cylinder 12 and the primary crushing cylinder 11 are in a same shape.
100491 A gap is formed between a lower inner wall of the secondary crushing cylinder 12 and a lower outer wall of the primary crushing cylinder 11; the secondary sieve pores have a pore size smaller than a pore size of the primary sieve pores, and the gap between the lower inner wall of the secondary crushing cylinder 12 and the lower outer wall of the primary crushing cylinder 11 is smaller than the pore size of the primary sieve pores.
[0050] When the grinding head 9 moves up and down in the primary crushing cylinder 11, the secondary crushing cylinder 12 rotates around the primary crushing cylinder 11.
100511 The grinding head 9 moves downward in the primary crushing cylinder 11, such that the original material between the grinding head 9 and the lower inner wall of the primary crushing cylinder 11 is squeezed and broken by the grinding head 9 and the lower inner wall of the primary crushing cylinder 11; [0052] Among the crushed raw material, materials with a particle size smaller than that of the primary sieve pore enters the gap between the lower inner wall of the secondary crushing cylinder 12 and the lower outer wall of the primary crushing cylinder 11, the secondary crushing cylinder 12 rotates around the primary crushing cylinder 11, such that the raw material in the gap is twisted and broken, and then crushed again * and materials whose particle size is smaller than that of the secondary sieve pore after secondary crushing are put into the slurry tank 1 through the secondary sieve pore [0053] During the refining, two staged breaking and crushing processes are conducted, and the processed materials are directly put into the slurry tank 1. There are no intermediate transfer steps in this process, thus ensuring that the refined materials are not contaminated by external substances.
[0054] As a further solution of this example, referring to FIG. 5 and FIG. 6, an upper inner wall of the powder-making cylinder 3 is provided with a circle of recess 15, an upper outer wall of the primary crushing cylinder 11 is provided with a circle of protrusion 13, and the protrusion 13 is fitted inside the recess 15.
100551 The primary crushing cylinder 11 is provided with a plurality of screw holes, the plurality of screw holes are equidistantly distributed along an outer periphery of the primary crushing cylinder 11, and the screw holes penetrate the recess 15; and a plurality of counter bores corresponding to the screw holes are arranged on the protrusion 13.
[0056] The powder-making cylinder 3 and the primary crushing cylinder 11 are fixed by bolts, and the bolts match threads of the screw holes and extend into the counter bores.
[0057] The fixation of the powder-making cylinder 3 and the primary crushing cylinder II is achieved by using the bolts, the screw holes and the counter bores; when the raw material is squeezed between the grinding head 9 and the lower inner wall of the primary crushing cylinder 11, a large axial shear force may be generated between the primary crushing cylinder 11 and the powder-making cylinder 3. Therefore, the protrusion 13 and the recess 15 are provided to share the axial bearing capacity of the bolt.
[0058] In summary, the bolts can provide supporting force for fixing the primary crushing cylinder 11 and the powder-making cylinder 3 in the tangential direction to prevent the powder-making cylinder 3 and the primary crushing cylinder 11 from rotating relative to each other. The protrusion 13 and the recess 15 can constrain the axial relative position between the powder-making cylinder 3 and the primary crushing cylinder 11 to avoid axial misalignment of the powder-making cylinder 3 and the primary crushing cylinder 11.
[0059] As a further solution of this example, referring to FIG. 5 and FIG. 6, a circle of track 16 is arranged on a lower inner wall of the powder-making cylinder 3, a plurality of carrier rollers 14 are arranged in a circumference at equal intervals on an outer periphery of the secondary crushing cylinder 12, the carrier rollers 14 are rotatably arranged on the outer wall of the secondary crushing cylinder 12, and the carrier rollers 14 are fitted in the track 16 in a rolling manner.
[0060] The fitting of the carrier roller 14 and the track 16 prevented the secondary crushing cylinder 12 and the powder-making cylinder 3 from axially deflecting, thereby ensuring the axial height consistency of the secondary crushing cylinder 12 and the primary crushing cylinder 11. Finally, the gap between the lower inner wall of the secondary crushing cylinder 12 and the lower outer wall of the primary crushing cylinder 11 is kept constant.
[0061] At the same time, the carrier roller 14 is fitted in the track 16 in a rolling manner to allow the secondary crushing cylinder 12 to rotate coaxially in the powder-making cylinder 3, that is, the secondary crushing cylinder 12 can rotate around the primary crushing cylinder 11.
100621 As a further solution of this example, referring to FIG. 1 and FIG. 5, a frame structure 4 is fixedly arranged on the sealing cover 2, a crankshaft 5 is horizontally and rotatably arranged on the frame structure 4, a bending portion at a middle of the crankshaft 5 is rotatably sleeved with an upper end of a connecting rod 7, and a lower end of the connecting rod 7 is rotatably fitted with an upper part of a driving rod 8 through a pin.
[0063] The grinding head 9 is fixed on a lower end of the driving rod 8, a support is fixed inside the powder-making cylinder 3, a grinding sleeve 10 is fixed in a center of the support, and the driving rod 8 penetrates the grinding sleeve 10 and is slidably fitted with the grinding sleeve 10. [0064] One end of the crankshaft 5 is connected to the output end of the gear motor 6 installed on one side of the frame structure 4.
[0065] The crankshaft 5 is driven to rotate by the gear motor 6. the crankshaft 5 drives the driving rod 8 through the connecting rod 7 to move up and down along the grinding sleeve 10, and finally drives the grinding head 9 to move up and down, such that the raw material between the grinding head 9 arid the lower inner wall of the primary crushing cylinder 11 is squeezed and broken by the grinding head 9 and the lower inner wall of the primary crushing cylinder 11. [0066] As a further solution of this example, referring to FIG 1 and FIG 5, a transmission rod 19 is further provided between the frame structure 4 and the powder-making cylinder 3, and the transmission rod 19 is arranged vertically, wherein a lower end and a central portion of the transmission rod 19 are rotatably fitted with an outer wall of the powder-making cylinder 3; an upper shaft journal of the transmission rod 19 is rotatably fitted with a bracket fixed on an inner side of the frame structure 4.
[0067] An upper end of the transmission rod 19 is connected to the crankshaft 5 through a bevel gear set, and a rotating gear 20 is fixed at a lower part of the transmission rod 19; a ring gear 22 is fixed on an outer wall of the secondary crushing cylinder 12, a notch 21 is arranged at a side of the powder-making cylinder 3 close to the rotating gear 20, and the rotating gear 20 crosses the notch 21 and meshes with the ring gear 22.
[0068] When the crankshaft 5 rotates, the bevel gear set drives the transmission rod 19 to rotate, and then drives the rotating gear 20 to rotate synchronously. Finally, the rotating gear 20 drives the ring gear 22 and the secondary crushing cylinder 12 to rotate around the primary crushing cylinder 11.
100691 In this embodiment, the rotation of the crankshaft 5 can simultaneously drive the grinding head 9 to move up and down and the secondary crushing cylinder 12 to rotate. In this way, the raw material is squeezed and crushed between the grinding head 9 and the primary crushing cylinder 1L Moreover, through the rotation of the secondary crushing cylinder 12 around the primary cnishing cylinder 11, the material entering the gap between the secondary crushing cylinder 12 and the primary crushing cylinder 11 is crushed again.
100701 With the help of mechanical cooperation, the raw materials are broken arid crushed twice in stages, with a high degree of coordination, and without the need for additional electrical system control, the failure rate is lower and the process is more reliable.
100711 The bevel gear set includes a driving gear 17 fixed on the upper end of the transmission rod 19 and a driven gear 18 fixed on the crankshaft 5. The driving gear 17 and the driven gear 18 mesh with each other.
[0072] As a further solution of this example, referring to FIG. 7 and FIG. 9, the mixing shaft 24 is rotatably arranged in the slurry tank 7, and both ends of the mixing shaft 24 penetrate the slurry tank 1 and are rotatably fitted with the slurry tank 1 in a sealed manner.
[0073] One end of the mixing shaft 24 is connected to an output end of a mixing motor 23 fixedly arranged on an outer wall of the slurry tank 1, and the mixing shaft 24 is provided with a plurality of sets of blades 25.
[0074] A lower part of the slurry tank 1 is in a shape of an inverted pagoda, and a gate valve 30 is arranged at a bottom of the slurry tank I. [0075] The mixing motor 23 can drive the mixing shaft 24 to rotate, and then drive the blades 25 to rotate in the slurry tank 1, such that the refined silicon nitride particles, aluminium oxide powder, pore-forming agent, and dispersant are evenly dispersed into the solvent obtained by mixing the cross-linking agent and the industrial ethanol.
[0076] As a further solution of this embodiment, the air pump 28 is fixedly arranged on the outer wall of the slurry tank I, an impeller shaft of the air pump 28 is coaxially fixed with a pumping shaft 27, and the pumping shaft 27 is connected to an other one end of the mixing shaft 24 through a transmission belt 26.
100771 An air outlet end of the air pump 28 penetrates the outer wall of the slurry tank 1, an air box is fixed on an inner wall of the slurry tank 1, and an air chamber is formed between the air box and the inner wall of the slurry tank I. [0078] The air outlet end of the air pump 28 is connected to the air chamber, a plurality of manifolds 29 are connected to the air chamber, and the manifolds 29 are close to the inner wall of the slurry tank I and extends to the bottom of the slurry tank I. 100791 The air pump 28 and the mixing shaft 24 and the like together form the blending component.
[0080] When the mixing shaft 24 rotates, the transmission belt 26 drives the pumping shaft 27 to rotate, which in turn drives the impeller shaft of the air pump 28 to rotate to pump argon or neon gas into the air chamber. The argon or neon gas in the air chamber is led to the bottom of the slurry tank 1 through the manifold 29, such that the slurry in the slurry tank I tumbles under the action of the air flow and the blades 25. In this way, the silicon nitride particles, aluminium oxide powder, pore-forming agent, and dispersant are evenly dispersed into the solvent obtained by mixing the cross-linking agent and the industrial ethanol. So that a uniform dispersion effect is achieved.
[0081] In addition, the pumped protective gas can also ensure the stability of the material properties of the slurry.
[0082] It should be noted that the raw material between the grinding head 9 and the lower inner wall of the primary crushing cylinder it can pass through the primary sieve pores under the extrusion of the grinding head 9. Therefore, when the raw materials in the primary crushing cylinder 11 are exhausted, the primary sieve pores may inevitably be tightly filled and blocked with the raw materials.
100831 In the same way, the secondary sieve pores can also be tightly filled and blocked with the material.
[0084] Obviously, during the crushing, the primary sieve pores and the secondary sieve pores are also filled and blocked with the materials, and the materials only pass through the primary sieve pores and the secondary sieve pores in one direction.
[0085] Therefore, during and after the breaking and crushing process, the protective gas in the slurry tank 1 cannot overflow through the primary sieve pores and the secondary sieve pores. Even if there has the overflow, there is only a small amount of the overflow.
[0086] Therefore, a positive pressure can be maintained inside the slurry tank 1. When the gate valve 30 is opened, due to the positive pressure in the slurry tank 1, the slurry in the slurry tank 1 can be quickly discharged and transferred to the mold 100871 A working process of the device of this embodiment is substantially as follows: [0088] The crankshaft 5 is driven to rotate by the gear motor 6; the crankshaft 5 drives the driving rod 8 through the connecting rod 7 to move up and down along the grinding sleeve 10, and finally drives the grinding head 9 to move up and down, such that the raw material between the grinding head 9 and the lower inner wall of the primary crushing cylinder 11 is squeezed and broken by the grinding head 9 and the lower inner wall of the primary crushing cylinder 11. 100891 The crankshaft 5 drives the driven gear 18 to rotate through the driving gear 17, thereby rotating the transmission rod 19, which in turn drives the rotating gear 20 to follow the rotation synchronously; ultimately, the rotating gear 20 drives the ring gear 22 and the secondary crushing cylinder 12 to rotate around the primary crushing cylinder 11, and the material entering the gap between the secondary crushing cylinder 12 and the primary crushing cylinder 11 is crushed again.
100901 With the help of mechanical cooperation, the raw materials are broken arid crushed twice in stages, with a high degree of coordination, and without the need for additional electrical system control, the failure rate is lower and the process is more reliable.
[0091] The mixing motor 23 can drive the mixing shaft 24 to rotate, and then drive the blade 25 to rotate in the slurry tank 1, such that the refined silicon nitride particles, aluminium oxide powder, pore-forming agent, and dispersant are evenly dispersed into the solvent obtained by mixing the cross-linking agent and the industrial ethanol; [0092] When the mixing shaft 24 rotates, the transmission belt 26 drives the pumping shaft 27 to rotate, which in turn drives the impeller shaft of the air pump 28 to rotate to pump argon or neon gas into the air chamber. The argon or neon gas in the air chamber is led to the bottom of the slurry tank 1 through the manifold 29, such that the slurry in the slurry tank 1 tumbles under the action of the air flow and the blades 25. In this way, the silicon nitride particles, aluminium oxide powder, pore-forming agent, and dispersant are evenly dispersed into the solvent obtained by mixing the cross-linking agent and the industrial ethanol. So that a uniform dispersion effect is achieved. The pumped protective gas can also ensure the stability of the material properties of the slurry.
100931 The above examples are exemplary rather than restrictive. Therefore, without departing from the spirit or basic characteristics of the present disclosure, technical solutions that can be implemented in other specific forms are included in the present disclosure.
Claims (1)
- WHAT IS CLAIMED IS: I. A preparation device of a silicon nitride wave-transparent material, wherein the preparation device is configured to produce a powder raw material of slurry, and mix a liquid raw material with the powder raw material to obtain the slurry in a preparation process of the silicon nitride wave-transparent material; wherein the preparation device comprises a slurry tank (1), a sealing cover (2) is arranged on an upper part of the slurry tank (1), a perforation is arranged in a center of the sealing cover (2), wherein a powder-making cylinder (3) is arranged on the perforation in a sealed manner, and the powder-making cylinder (3) communicates with an interior of the slurry tank (1) through the perforation; wherein a refining mechanism is provided in the powder-making cylinder (3), the refining mechanism is configured to refine silicon nitride particles, aluminium oxide powder, a pore-forming agent, and a dispersant, and wherein a blending component is provided in the slurry tank (1), the blending component is configured to uniformly disperse the silicon nitride particles, the aluminium oxide powder, the pore-forming agent, and the dispersant that are refined into a solvent obtained by mixing a cross-linking agent and industrial ethanol 2. The preparation device of a silicon nitride wave-transparent material according to claim 1, wherein the refining mechanism comprises: a primary crushing cylinder (11) fixedly arranged in the powder-making cylinder (3), wherein a plurality of primary sieve pores are evenly arranged in a lower part of the primary crushing cylinder (11); a grinding head (9) movably arranged in the primary crushing cylinder (11); the grinding head (9) is movable up and down in the primary crushing cylinder (11) to grind the silicon nitride particles, the aluminium oxide powder, the pore-forming agent, and the dispersant in conjunction with a lower inner wall of the primary crushing cylinder (11); and a gap is formed between an outer periphery of the grinding head (9) and the lower inner wall of the primary crushing cylinder (11), so as to allow an original material poured from an upper port of the powder-making cylinder (3) to enter the primary crushing cylinder (11); a secondary crushing cylinder (12) rotatably arranged outside the primary crushing cylinder (11), wherein a plurality of secondary sieve pores are evenly arranged in a lower part of the primary crushing cylinder (11), and the secondary crushing cylinder (12) and the primary crushing cylinder (11) are in a same shape; wherein a gap is formed between a lower inner wall of the secondary crushing cylinder (12) and a lower outer wall of the primary crushing cylinder (11); the secondary sieve pores have a pore size smaller than a pore size of the primary sieve pores, and the gap between the lower inner wall of the secondary crushing cylinder (12) and the lower outer wall of the primary crushing cylinder (11) is smaller than the pore size of the primary sieve pores; and wherein when the grinding head (9) moves up and down in the primary crushing cylinder (11), the secondary crushing cylinder (12) rotates around the primary crushing cylinder (11).3 The preparation device of a silicon nitride wave-transparent material according to claim 2, wherein a frame structure (4) is fixedly arranged on the sealing cover (2), a crankshaft (5) is horizontally and rotatably arranged on the frame structure (4), a bending portion at a middle of the crankshaft (5) is rotatably sleeved with an upper end of a connecting rod (7), and a lower end of the connecting rod (7) is rotatably fitted with an upper part of a driving rod (8) through a pin, and the grinding head (9) is fixed on a lower end of the driving rod (8), a support is fixed inside the powder-making cylinder (3), a grinding sleeve (10) is fixed in a center of the support, and the driving rod (8) penetrates the grinding sleeve (10) and is slidably fitted with the grinding sleeve (10).4 The preparation device of a silicon nitride wave-transparent material according to claim 3, wherein a transmission rod (19) is further provided between the frame structure (4) and the powder-making cylinder (3), and the transmission rod (19) is arranged vertically, wherein a lower end and a central portion of the transmission rod (19) are rotatably fitted with an outer wall of the powder-making cylinder (3); an upper shaft journal of the transmission rod (19) is rotatably fitted with a bracket fixed on an inner side of the frame structure (4), and an upper end of the transmission rod (19) is connected to the crankshaft (5) through a bevel gear set, and a rotating gear (20) is fixed at a lower part of the transmission rod (19); a ring gear (22) is fixed on an outer wall of the secondary crushing cylinder (12), a notch (21) is arranged at a side of the powder-making cylinder (3) close to the rotating gear (20), and the rotating gear (20) crosses the notch (21) and meshes with the ring gear (22) 5. The preparation device of a silicon nitride wave-transparent material according to claim 1, wherein the blending component comprises an air pump (28) and a mixing shaft (24), the mixing shaft (24) is rotatably arranged in the slurry tank (7), and both ends of the mixing shaft (24) penetrate the slurry tank (1) and are rotatably fitted with the slurry tank (1) in a sealed manner; one end of the mixing shaft (24) is connected to an output end of a mixing motor (23) fixedly arranged on an outer wall of the slurry tank (1), and the mixing shaft (24) is provided with a plurality of sets of blades (25); and a lower part of the slurry tank (1) is in a shape of an inverted pagoda, and a gate valve (30) is arranged at a bottom of the slurry tank (1).6. The preparation device of a silicon nitride wave-transparent material according to claim 5, wherein the air pump (28) is fixedly arranged on the outer wall of the slurry tank (1), an impeller shaft of the air pump (28) is coaxially fixed with a pumping shaft (27), and the pumping shaft (27) is connected to an other one end of the mixing shaft (24) through a transmission belt (26); an air outlet end of the air pump (28) penetrates the outer wall of the slurry tank (1), an air box is fixed on an inner wall of the slurry tank (1), and an air chamber is formed between the air box and the inner wall of the slurry tank (1); and the air outlet end of the air pump (28) is connected to the air chamber, a plurality of manifolds (29) are connected to the air chamber, and the manifolds (29) are close to the inner wall of the slurry tank (1) and extends to the bottom of the slurry tank (1) 7. The preparation device of a silicon nitride wave-transparent material according to claim 2, wherein a circle of track (16) is arranged on a lower inner wall of the powder-making cylinder (3), a plurality of carrier rollers (14) are arranged in a circumference at equal intervals on an outer periphery of the secondary crushing cylinder (12), the carrier rollers (14) are rotatably arranged on the outer wall of the secondary crushing cylinder (12), and the carrier rollers (14) are fitted in the track (16) in a rolling manner.8. The preparation device of a silicon nitride wave-transparent material according to claim 2, wherein an upper inner wall of the powder-making cylinder (3) is provided with a circle of recess (15), an upper outer wall of the primary crushing cylinder (11) is provided with a circle of protrusion (13), and the protrusion (13) is fitted inside the recess (15); the primary crushing cylinder (11) is provided with a plurality of screw holes, the plurality of screw holes are equidistantly distributed along an outer periphery of the primary crushing cylinder (11), and the screw holes penetrate the recess (15); and a plurality of counter bores corresponding to the screw holes are arranged on the protrusion (13); and the powder-making cylinder (3) and the primary crushing cylinder (11) are fixed by bolts, and the bolts match threads of the screw holes and extend into the counter bores.9. A silicon nitride wave-transparent material, comprising the following raw materials: 35 parts of a cross-linking agent, 30 parts of industrial ethanol, 25 parts of silicon nitride particles, 5 parts of aluminium oxide powder, 3 parts of a pore-forming agent, and 2 parts of a dispersant.10. A preparation process of the silicon nitride wave-transparent material according to claim 9, comprising the following steps: sl, production of a powder raw material of slurry: refining the silicon nitride particles, the aluminium oxide powder, the pore-forming agent, and the dispersant; s2, blending and preparation of the slurry: putting the refined powder raw material of the slurry into a container containing deionized water and the industrial ethanol to allow mixing; dispersing the silicon nitride, the aluminium oxide, and the pore-forming agent evenly into a solvent obtained by mixing the cross-linking agent and the industrial ethanol under an action of the dispersant; and introducing a protective gas into the container while mixing; s3, slurry discharging and forming: transferring the prepared slurry from the container into a mold to form a layered structure, and controlling a thickness of each layer to form a prefabricated material blank; and s4, sintering and molding: stacking the prefabricated material blank with different layered structures according to predetermined layer levels, and conducting sintering in a nitrogen environment at a pressure of 1 MiPa to 1.5 MPa and at a temperature of 1,500V to 1,950°C for 2 h to 5 h.
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| PCT/CN2023/103706 WO2024082697A1 (en) | 2022-10-17 | 2023-06-29 | Silicon nitride wave-transmitting material, preparation process and preparation apparatus |
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| CN103274696A (en) * | 2013-04-19 | 2013-09-04 | 北京中材人工晶体研究院有限公司 | Heat wave-transmission porous ceramic material and preparation method thereof |
| CN108033801A (en) * | 2017-11-23 | 2018-05-15 | 中国人民解放军国防科技大学 | Silicon nitride nanowire reinforced porous silicon nitride composite material and preparation method thereof |
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| CN103274696A (en) * | 2013-04-19 | 2013-09-04 | 北京中材人工晶体研究院有限公司 | Heat wave-transmission porous ceramic material and preparation method thereof |
| US10968139B1 (en) * | 2017-07-18 | 2021-04-06 | ATC Materials, Inc. | Moldable silicon nitride green-body composite and reduced density silicon nitride ceramic process |
| CN108033801A (en) * | 2017-11-23 | 2018-05-15 | 中国人民解放军国防科技大学 | Silicon nitride nanowire reinforced porous silicon nitride composite material and preparation method thereof |
| CN115626839A (en) * | 2022-10-17 | 2023-01-20 | 衡阳凯新特种材料科技有限公司 | Silicon nitride wave-transparent material, preparation process and preparation device |
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