CN115321984A - Silicon carbide thin-wall pipe and manufacturing method and equipment thereof - Google Patents
Silicon carbide thin-wall pipe and manufacturing method and equipment thereof Download PDFInfo
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- CN115321984A CN115321984A CN202211033485.5A CN202211033485A CN115321984A CN 115321984 A CN115321984 A CN 115321984A CN 202211033485 A CN202211033485 A CN 202211033485A CN 115321984 A CN115321984 A CN 115321984A
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 123
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 109
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 18
- 239000000314 lubricant Substances 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 239000002270 dispersing agent Substances 0.000 claims abstract description 11
- 239000004014 plasticizer Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims description 174
- 239000007788 liquid Substances 0.000 claims description 93
- 238000003860 storage Methods 0.000 claims description 44
- 238000005192 partition Methods 0.000 claims description 28
- 238000007789 sealing Methods 0.000 claims description 20
- 238000005245 sintering Methods 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000012530 fluid Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 16
- 239000011812 mixed powder Substances 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 238000000465 moulding Methods 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 3
- 239000005642 Oleic acid Substances 0.000 claims description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 3
- 238000003483 aging Methods 0.000 claims description 3
- 238000005238 degreasing Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 3
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 3
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 3
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical group OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 230000000052 comparative effect Effects 0.000 description 12
- 238000007599 discharging Methods 0.000 description 9
- 239000000919 ceramic Substances 0.000 description 7
- 238000005260 corrosion Methods 0.000 description 7
- 230000007797 corrosion Effects 0.000 description 7
- 239000013078 crystal Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
- 229910021431 alpha silicon carbide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000004579 marble Substances 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C04B35/56—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 carbides or oxycarbides
- C04B35/565—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 carbides or oxycarbides based on silicon carbide
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Abstract
The application relates to the field of material preparation, and particularly discloses a silicon carbide thin-wall tube and a manufacturing method and equipment thereof. The silicon carbide thin-wall pipe comprises the following raw materials: silicon carbide; the plasticizer is used in an amount of 10-13wt% of the silicon carbide; the new parison methyl CMC-BL, the consumption of said new parison methyl CMC-BL is 0.2-2wt% of the carborundum; the lubricant accounts for 1-4wt% of the silicon carbide; the using amount of the dispersing agent is 10-20wt% of the silicon carbide; the amount of water is 20-30wt% of the silicon carbide. The silicon carbide thin-wall tube with the wall thickness of less than 0.3mm can be prepared, and the silicon carbide thin-wall tube is excellent in performance and high in uniformity; the non-roundness of the silicon carbide thin-wall pipe is less than 0.05mm, the straightness is less than 1.0mm/m, the wall thickness difference is less than 0.03mm, the silicon carbide thin-wall pipe is convenient to assemble, and the wear-resisting and corrosion-resisting properties are excellent.
Description
Technical Field
The application relates to the field of material preparation, in particular to a silicon carbide thin-wall tube and a manufacturing method and equipment thereof.
Background
The silicon carbide ceramic has the excellent performances of stable chemical performance, high thermal conductivity, small thermal expansion coefficient, high hardness, good wear resistance and corrosion resistance and the like, so that the silicon carbide ceramic is widely applied to heat exchange systems in harsh environments such as high temperature, corrosion and the like.
In addition, the thin-walled silicon carbide ceramic heat exchange tube has the advantages of thin wall, high heat exchange efficiency and the like, and thus becomes the mainstream of the development of the current heat exchanger.
However, the wall thickness of the silicon carbide thin-wall tube produced in China at present is generally between 1mm and 3mm, and in order to expand the application field of the silicon carbide tube, how to manufacture the high-performance thin-wall silicon carbide ceramic tube with the wall thickness of less than 0.3mm becomes a difficult problem to be solved urgently.
Disclosure of Invention
In order to manufacture a high-performance thin-wall silicon carbide ceramic tube with the wall thickness of less than 0.3mm, the application provides a silicon carbide thin-wall tube and a manufacturing method and equipment thereof.
In a first aspect, the present application provides a silicon carbide thin-walled tube, which adopts the following technical scheme:
the silicon carbide thin-wall pipe comprises the following raw materials: silicon carbide; the plasticizer accounts for 10-13wt% of the silicon carbide; the new parison methyl CMC-BL, the consumption of said new parison methyl CMC-BL is 0.2-2wt% of the silicon carbide; a lubricant, wherein the amount of the lubricant is 1-4wt% of the silicon carbide; the using amount of the dispersing agent is 10-20wt% of the silicon carbide; and the amount of the water is 20-30wt% of the silicon carbide.
By adopting the technical scheme, the silicon carbide thin-wall pipe with the wall thickness of less than 0.3mm can be prepared, and the silicon carbide thin-wall pipe has excellent performance and high uniformity; the non-roundness of the silicon carbide thin-wall pipe is less than 0.05mm, the straightness is less than 1.0mm/m, the wall thickness difference is less than 0.03mm, the silicon carbide thin-wall pipe is convenient to assemble, and the wear resistance and corrosion resistance are excellent.
Optionally, the plasticizer is hydroxypropyl methylcellulose, the lubricant is at least one of glycerol and oleic acid, and the dispersant is polyethylene glycol.
In a second aspect, the application provides a preparation method of a silicon carbide thin-walled tube, which adopts the following technical scheme:
a preparation method of a silicon carbide thin-wall tube comprises the following steps:
mixing: mixing silicon carbide, plasticizer and novel blank methyl CMC-BL to obtain mixed powder; uniformly mixing water, a lubricant and a dispersant to obtain a mixed solution, uniformly mixing the mixed solution and the mixed powder, carrying out vacuum mixing, and sealing and ageing to obtain aged mud;
molding: extruding and molding the aged pug, and drying to obtain a thin-wall tube blank;
and (3) high-temperature sintering: and sintering the thin-walled tube blank to obtain the silicon carbide thin-walled tube.
Optionally, in the molding step, after the aged pug is extruded and molded, air floatation support is carried out, and the air pressure is 0.1-0.6Mpa; and drying by microwave at 50-80 deg.C.
By adopting the technical scheme, the deformation degree of the green body can be reduced by adopting air floatation support and simultaneously controlling the drying temperature, so that the silicon carbide thin-wall pipe with more excellent performance can be obtained.
Optionally, the high-temperature sintering operation includes the following steps:
degreasing: heating to 600-1100 deg.C under vacuum micro-negative pressure, heating at a rate of 1-3 deg.C/min, and maintaining for 10-60min;
and (3) heating: heating to 1100-1900 deg.c at a rate of 3-10 deg.c/min and maintaining for 20-30min;
and (3) sintering: filling argon to 10-50KPa, heating to 1900-2100 deg.C, heating at 1-5 deg.C/min, and maintaining for 10-55min;
and (3) cooling: cooling to 1500-1800 deg.C, maintaining the temperature for 30-60min, and cooling to room temperature to obtain silicon carbide thin-wall tube.
By adopting the technical scheme, in the high-temperature sintering process, a carbon source in the green body can react with liquid-phase silicon to generate beta-silicon carbide, and the beta-silicon carbide is dispersed in silicon liquid or adsorbed on alpha-silicon carbide; along with the sintering process, small-sized silicon carbide particles are continuously migrated, dissolved, separated out and aggregated in the silicon liquid to grow into large-sized silicon carbide crystal particles, and the silicon liquid can fill redundant gaps, so that the obtained silicon carbide thin-wall pipe is very compact and has good service performance. In the application, the proper temperature, the proper heat preservation time and the proper temperature rise rate are selected through controlling the sintering conditionsAnd simultaneously sintering the silicon carbide crystal grains in stages so that the growth process of the silicon carbide crystal grains is more stable, and the wall thickness can be obtained<0.3mm thin-walled tube of silicon carbide, and the density of the thin-walled tube of silicon carbide is more than 3.10g/cm 3 The silicon carbide thin-wall pipe has good wear resistance and corrosion resistance.
In a third aspect, the present application provides a device for a preparation method of a silicon carbide thin-walled tube, which adopts the following technical scheme:
the equipment is used for the preparation method of the silicon carbide thin-wall tube, and is used for mixing liquid and mixed powder; the equipment comprises a mixing tank body, wherein a partition plate is arranged on the inner wall of the mixing tank body, the mixing tank body is divided into a liquid storage area and a mixing area from bottom to top by the partition plate, the inner wall of the mixing tank body, which is positioned in the mixing area, is provided with the partition plate, and the mixing area is divided into mixing cavities which are arranged from bottom to top by the partition plate; a dividing baffle is arranged between the inner wall of the mixing tank body positioned in the liquid storage area and the partition plate, and the dividing baffle divides the liquid storage area into at least two liquid storage cavities; a feeding pipe communicated with each liquid storage cavity is arranged on the mixing tank body, a material guide pipe is arranged between each liquid storage cavity and the mixing cavity adjacent to the liquid storage area, and a material guide assembly is arranged in each liquid storage cavity; a material conveying assembly for conveying materials in the lower mixing cavity to the upper mixing cavity is arranged between every two adjacent mixing cavities, and a mixing device is arranged in each mixing cavity; the mixing tank body is provided with a discharge assembly communicated with the mixing cavity at the top.
By adopting the technical scheme, when the mixing cavity above the mixing cavity is not filled with materials, the materials are injected into the mixing cavity below and adjacent mixing cavities above the conveying assembly. Meanwhile, when the material guide assembly does not contain materials in the mixing cavity at the lowest part, the materials in the liquid storage cavity are conveyed into the mixing cavity at the lowest part. Therefore, the materials are continuously mixed in the three mixing cavities, the total mixing time is the same, the materials can be fully and uniformly mixed, and the powder materials are uniformly dispersed in the liquid.
Optionally, the material guide assembly includes a piston plate and a closing plate, the piston plate is slidably disposed on the wall of the liquid storage cavity along a vertical direction, a vertical side wall of the piston plate is hermetically connected with the wall of the mixing cavity, the mixing cavity is divided into an upper power cavity and a lower passive cavity by the piston plate, the bottom end of the material guide pipe penetrates through the piston plate and is slidably connected with the piston plate, and an outer wall of the material guide pipe is hermetically connected with the piston plate; a fluid pipe communicated with the power cavity is connected to the mixing tank body, and the fluid pipe is connected with a retraction assembly for fluid to enter and exit; the mixing tank body is connected with a pressure balancing piece communicated with the passive cavity; the sealing plate is arranged on the inner wall of the material guide pipe in a sliding mode, a one-way valve is arranged on the material guide pipe, the sealing plate is located between the one-way valve and the piston plate, and a driving assembly used for driving the sealing plate to slide is arranged on the material guide pipe.
By adopting the technical scheme, the pressure balance piece is opened, so that materials can be normally input into the liquid storage cavity; the pressure balance piece is closed, fluid is added into the power cavity through the fluid pipe, the piston plate moves downwards under the action of pressure, the material can be pressed into the material guide pipe, the driving assembly drives the sealing plate to move, the material guide groove is opened, and the material can enter the mixing cavity. When materials are added into the liquid storage cavity next time, the retraction assembly is used for pumping out the fluid in the power cavity, so that the piston plate can move upwards, and sufficient space is provided for the materials.
Optionally, the driving assembly includes a base block, a driving gear, a driving toothed plate, a reversing gear, a reversing toothed plate and an elastic pull rope, the base block is relatively disposed on the side wall of the material guide pipe, a sliding chute is disposed at one end of the base block, which is far away from the side wall of the material guide pipe, and is connected with the sliding chute in a sliding manner, a driving cavity is disposed in the base block and is communicated with the sliding chute, a linkage toothed plate is disposed at one end of the sealing block, which extends into the driving cavity, and is rotatably disposed on the wall of the driving cavity, the driving gear is engaged with the linkage toothed plate, a matching gear is further rotatably connected to the wall of the driving cavity, and the matching gear is engaged with the linkage gear; the driving toothed plate is arranged on the wall of the driving cavity in a sliding manner, and the driving toothed plate is meshed with the matching gear; a positioning spring is arranged between the driving gear and the wall of the driving cavity; the driving toothed plate is provided with a reversing plate, and the reversing plate extends out of the material guide pipe and is connected with the material guide pipe in a sliding manner; a base plate is arranged on the cavity wall of the power cavity, a reversing rotating wheel is connected to the base plate in a rotating mode, a reversing toothed plate is arranged on the base plate in a sliding mode along the vertical direction, a reversing rope is connected between one end, extending out of the material guide pipe, of the reversing plate and the top end of the reversing toothed plate, and the reversing rope is abutted to the reversing rotating wheel; the reversing gear is rotatably arranged on the base plate and meshed with the reversing toothed plate; the reversing gear is coaxially connected with a retracting wheel, a coil spring is arranged between the retracting wheel and the side wall of the reversing gear, one end of the elastic pull rope is fixedly connected with the retracting wheel, and the other end of the elastic pull rope bypasses the retracting wheel and is fixedly connected with the piston plate.
Through taking above-mentioned technical scheme, along with the piston plate moves down, the elasticity stay cord can drive and receive and release the wheel rotation, receive and release the wheel and drive the reversing gear and rotate, reversing gear and reversing tooth plate meshing, the reversing rope pulls the drive pinion rack and removes, drive pinion rack and cooperation gear meshing, cooperation gear and linkage pinion rack meshing, the linkage pinion rack can drive the closing plate and remove and open passage, convenient and fast. And in the process of opening the material guide pipe by the closing plate, the positioning spring and the coil spring are stretched, so that when the piston plate moves upwards, the coil spring can drive the retraction wheel to rotate reversely, and the positioning spring can drive the driving toothed plate to reset in a matched manner, so that the closing plate automatically closes the material guide pipe. And after the elastic pull ropes are completely rotated from the retractable wheels, the elastic pull ropes can be elastically deformed, so that the piston plate can continue to move downwards, and the quantity of the materials entering the mixing cavity can be conveniently controlled.
Optionally, the material conveying assembly comprises a material conveying pipe, a connecting pipe and a material conveying pipe, the material conveying pipe is arranged between adjacent mixing chambers, and the material conveying pipe penetrates through the partition plate and is connected with the partition plate in a sealing manner; the connecting pipe is connected between the bottom end and the top end of the two adjacent conveying pipes, the two material walking pipes are connected to the connecting pipe, the connecting pipe is connected with a power pump, the power pump is located between the two material walking pipes, a first control valve is arranged on each material walking pipe, two second control valves are arranged on the connecting pipe, and the power pump and the material walking pipes are located between the two second control valves.
By adopting the technical scheme, taking three mixing chambers as an example, the second control valve adjacent to the uppermost mixing chamber and the first control valve on the feeding pipe adjacent to the lowermost mixing chamber are closed, so that the material in the lowermost mixing chamber forms a passage through the material guide pipe, the connecting pipe and the feeding pipe adjacent to the uppermost mixing chamber, and the material in the lowermost mixing chamber can be added into the middle mixing chamber by using the power pump. And closing a second control valve adjacent to the bottommost mixing cavity and a first control valve on the material feeding pipe adjacent to the uppermost mixing cavity, wherein the material feeding pipe, the connecting pipe and the material guiding pipe adjacent to the bottommost mixing cavity form a passage, so that the materials in the middle mixing cavity can be added into the uppermost mixing cavity by using the power pump.
Optionally, the mixing device includes a heater mounted on the mixing tank body and a rotating base shaft rotatably connected between the partition plates, a stirring blade is mounted on the rotating base shaft, a motor is mounted on the top wall of the mixing tank body, and the motor is fixedly connected with the top end of the rotating base shaft.
In summary, the present application includes at least one of the following beneficial technical effects:
1. due to the wall thickness<The wall thickness of the silicon carbide thin-wall pipe with the thickness of 0.3mm is much thinner than that of the common silicon carbide thin-wall pipe with the wall thickness of 1-3mm, and the wall thickness is much thinner<The difficulty in preparing the silicon carbide thin-wall tube with the thickness of 0.3mm is also bound to be higher; firstly, the wall thickness of the silicon carbide thin-wall pipe is thinned, compared with the thicker silicon carbide thin-wall pipe, the uniformity of the wall thickness is more difficult to control, how to control the form of the silicon carbide thin-wall pipe is good, and meanwhile, the silicon carbide thin-wall pipe still has good service performances such as wear resistance, corrosion resistance and the like, and is a very complicated and important process; the inventor conducts a great deal of research and starts from both experimental and theoretical aspectsWhen a specified amount of novel blank methyl CMC-BL is added, the other components are matched, and the sintering process is well controlled, the silicon carbide thin-wall tube with excellent performance can be prepared, the wall thickness is less than 0.3mm, the uniformity of the tube body is excellent, and the silicon carbide thin-wall tube is convenient to assemble; and the density of the silicon carbide thin-wall pipe is 3.10g/cm 3 The wear resistance and corrosion resistance are also very excellent; the inventors believe that this may be a composition and sintering work of each specified amount, affecting the growth of the silicon carbide crystal grains, suitable composition and suitable sintering conditions, so that the present application can produce a thin-walled tube of silicon carbide with excellent properties;
2. in order to further improve the performance of the silicon carbide thin-walled tube and reduce the deformation of the silicon carbide thin-walled tube, the application provides the mixing equipment which can uniformly mix all the components together, so that the performance of the silicon carbide thin-walled tube is further improved.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus used in a method for producing a thin-walled tube of silicon carbide according to example 13 of the present application.
Fig. 2 isbase:Sub>A sectional view taken along linebase:Sub>A-base:Sub>A of fig. 1.
Fig. 3 is an enlarged view at B in fig. 2.
Fig. 4 is a schematic diagram of a driving assembly according to embodiment 13 of the present application.
Fig. 5 is a schematic view of a material delivery assembly according to an embodiment 13 of the present application.
Fig. 6 is an enlarged view at C in fig. 5.
Description of reference numerals: 1. a mixing tank body; 11. a separator plate; 12. a liquid storage area; 13. a mixing zone; 14. a partition plate; 15. a mixing chamber; 151. a power cavity; 152. a passive cavity; 16. dividing a baffle; 17. a liquid storage cavity; 18. a feed pipe; 19. a material guide pipe; 191. a through groove; 2. a material guiding assembly; 21. a piston plate; 22. a closing plate; 23. a fluid pipe; 24. a fifth control valve; 25. a base pipe; 26. a one-way valve; 3. a material conveying component; 31. a delivery pipe; 32. a connecting pipe; 33. a feeding pipe; 34. a power pump; 35. a second control valve; 36. a first control valve; 4. a mixing device; 41. a heater; 42. rotating the base shaft; 43. a stirring sheet; 44. a motor; 5. a discharge assembly; 51. a discharge pipe; 52. a discharge pump; 6. a retraction assembly; 61. collecting and releasing the pipe; 62. a third control valve; 7. a pressure balance member; 71. a balance tube; 72. a fourth control valve; 8. a drive assembly; 81. a base block; 811. a sliding groove; 812. a drive chamber; 82. a drive gear; 83. a driving toothed plate; 831. a positioning spring; 84. a reversing gear; 841. a substrate; 842. a reversing rope; 843. a retracting wheel; 845. a coil spring; 85. a reversing toothed plate; 86. an elastic pull rope; 87. a linkage toothed plate; 88. a mating gear; 89. a reversing plate; 891. and 4, reversing the rotating wheel.
Detailed Description
The present application is described in further detail below with reference to the accompanying drawings.
Example 1
The silicon carbide thin-wall pipe comprises the following raw materials: silicon carbide; plasticizer, wherein the dosage of the plasticizer is 12wt% of the silicon carbide; the novel blank methyl CMC-BL is used in an amount of 1.3wt% of the silicon carbide; a lubricant, wherein the amount of the lubricant is 3.2wt% of the silicon carbide; dispersing agent, the dosage of the dispersing agent is 14.3wt% of the silicon carbide; the amount of water used was 27.6wt% of the silicon carbide.
Wherein the plasticizer is hydroxypropyl methylcellulose, the lubricant is glycerol, the dispersant is polyethylene glycol, and the molecular weight is 1100.
A preparation method of a silicon carbide thin-wall tube comprises the following steps:
mixing: mixing silicon carbide, a plasticizer and the novel blank with methyl CMC-BL to obtain mixed powder; uniformly mixing water, a lubricant and a dispersant to obtain a mixed solution, uniformly mixing the mixed solution and the mixed powder, carrying out vacuum mixing twice, and sealing and ageing for 20 hours to obtain aged pug;
molding: extruding and molding the aged pug, and then carrying out air floatation support on the molded pipe body, wherein radial and axial air pressure suspension support is adopted, and the air pressure is 0.4Mpa; then, microwave drying is carried out at the drying temperature of 70 ℃, and finally a thin-wall tube blank is obtained;
and (3) high-temperature sintering: the sintering method of the thin-walled tube blank specifically comprises the following steps:
degreasing: heating to 900 ℃ under a vacuum micro negative pressure (-0.1 MPa), wherein the heating rate is 2 ℃/min, and the temperature is kept for 50min;
and (3) heating: heating to 1500 ℃, heating rate is 6 ℃/min, and keeping the temperature for 26min;
and (3) sintering: filling argon to 30KPa, heating to 2000 ℃, heating at a rate of 3 ℃/min, and keeping the temperature for 30min;
and (3) cooling: cooling to 1600 ℃, preserving heat for 40min, and finally cooling to room temperature to obtain the silicon carbide thin-wall tube.
Examples 2 to 3
Examples 2-3 differ from example 1 in that: the amounts of the components used in examples 2-3 were different from those of example 1, and are shown in Table 1.
TABLE 1 compositional content scale of examples 1-3 (in mass percent compared to the amount of silicon carbide)
Example 6
Example 6 differs from example 1 in that: the lubricant is oleic acid.
Examples 7 to 12
Examples 7-12 differ from example 1 in that: the preparation process parameters of examples 7 to 12 were different from those of example 1, and specifically shown in tables 2 and 3
TABLE 2 preparation Process parameters Table for example 1 and examples 7-8
TABLE 2 preparation of examples 1 and 9 to 12 Table of parameters of the preparation process (temperature in deg.C, temperature rise rate in deg.C/min, holding time in min, argon pressure in KPa)
Example 13
Example 13 provides an apparatus for use in a method of making a silicon carbide thin walled tube.
As shown in fig. 1 and 2, the equipment for the preparation method of the silicon carbide thin-wall tube comprises a mixing tank body 1, wherein a partition plate 11 is fixedly connected to the inner wall of the mixing tank body 1, the partition plate 11 is horizontally arranged and divides the mixing tank body 1 into a liquid storage area 12 and a mixing area 13, the liquid storage area 12 is positioned below the mixing area 13, and the tank body diameter of the liquid storage area 12 is larger than that of the mixing area 13; the inner wall of the mixing tank body 1 in the mixing area 13 is fixedly connected with a partition plate 14, the partition plate 14 can be one, two, three or the like, and the number of the partition plates 14 in the embodiment is two; the two partition plates 14 are both horizontally arranged and divide the mixing area 13 into three mixing cavities 15 which are arranged from bottom to top; the mixing tank body 1 is located fixedly connected with between the lateral wall of the liquid storage area 12 and the bottom wall of the partition plate 11 and divides the baffle 16, the number of the divided baffles 16 can be one, two, etc., the divided baffle 16 in the embodiment has one, the divided baffle 16 is vertically arranged and divides the liquid storage area 12 into two mutually independent liquid storage cavities 17.
The bottom end of the mixing tank body 1 is connected with two feeding pipes 18, and each liquid storage cavity 17 is communicated with one feeding pipe 18; the partition plate 11 is fixedly connected with two material guide pipes 19, the top ends of the material guide pipes 19 extend into the mixing cavity 15 at the lowest part, the bottom ends of the material guide pipes 19 extend into the bottom ends of the corresponding liquid storage cavities 17, and each liquid storage cavity 17 corresponds to one material guide pipe 19; meanwhile, the material guide assembly 2 is arranged in each liquid storage cavity 17, and the material guide assembly 2 can convey materials in the liquid storage cavities 17 to the mixing cavity 15 at the lowest part. Each partition 14 is provided with a feed conveyor assembly 3, the feed conveyor assembly 3 being adapted to convey material from a lower mixing chamber 15 to an upper adjacent mixing chamber 15, and each mixing chamber 15 being provided with a mixing device 4. In addition, the top end of the mixing tank body 1 is connected with a discharging component 5, and the discharging component 5 is communicated with the uppermost mixing cavity 15.
The mixed solution is divided into two parts, wherein one part is mixed with the mixed powder in advance. Then, the two mixed liquids are delivered to the corresponding liquid storage cavities 17, and then the material guiding assembly 2 delivers the mixed liquids to the lowermost mixing cavity 15 through the material guiding pipe 19, wherein T time is required for adding the mixed liquids in the liquid storage pipes to a proper amount, and T time is required for transferring a specified amount of the mixed liquids from the liquid storage cavities 17 to the lowermost mixing cavity 15. After the mixed liquid is mixed in the mixing cavity 15 at the bottom for a period of time, the material guiding assembly 2 conveys the mixed liquid into the mixing cavity 15 at the middle, wherein the mixing time is T1, and the conveying time is T1; after the mixed liquid is mixed in the middle mixing chamber 15 for a period of time, the mixed liquid is completely conveyed to the uppermost mixing chamber 15, wherein the mixing time is T2, and the conveying time is T2. The mixed liquid is mixed for a period of time in the mixing chamber 15 at the top, and finally the discharging component 5 outputs the mixed liquid completely, wherein the mixing time is T3, and the discharging time is T3. In the embodiment, the mixed liquid is intermittently injected into the two liquid storage cavities 17, the interval time is greater than or equal to T + T, T is greater than or equal to T1+ T1, T1 is greater than or equal to T2+ T2, and T2 is greater than or equal to T3+ T3, and in summary, when there is no mixed liquid in the adjacent upper mixing cavity 15, the mixed liquid is injected into the upper mixing cavity 15, so that the mixed liquid is continuously mixed in the three mixing cavities 15 and the total mixing time is the same. Finally, the two mixed solutions can be uniformly mixed together, the mixed powder can be uniformly dispersed in the mixed solution, and in the mixed solution of different batches, the dispersion condition of the mixed powder in the mixed solution is approximate, so that the uniformity of the performance of the silicon carbide thin-wall tube is improved.
As shown in fig. 1, 2 and 3, the material guiding assembly 2 in this embodiment includes a piston plate 21 and a closing plate 22, the piston plate 21 and the liquid storage cavity 17 are arranged in a one-to-one correspondence manner, the piston plate 21 is slidably arranged on the cavity wall of the liquid storage cavity 17 along the vertical direction, the vertical side wall of the piston plate 21 is attached to and sealed with the cavity wall of the mixing cavity 15, the mixing cavity 15 is divided into a power cavity 151 and a passive cavity 152 which are independent of each other by the piston plate 21, the passive cavity 152 is located below the power cavity 151, and the passive cavity 152 is communicated with the feeding pipe 18; and the bottom end of the material guiding pipe 19 passes through the piston plate 21 and is connected with the piston plate 21 in a sliding way, and the outer wall of the material guiding pipe 19 is connected with the piston plate 21 in a sealing way. A fluid pipe 23 communicated with the power chamber 151 is connected to the mixing tank body 1, a fifth control valve 24 is installed on the fluid pipe 23, and the fluid pipe 23 is used for conveying liquid or gas, and the fluid in this embodiment is liquid. The fluid pipe 23 is connected with a retraction assembly 6; the retraction assembly 6 comprises a retraction pipe 61 connected to the pipe wall of the fluid pipe 23 extending out of the mixing tank body 1, and a third control valve 62 is mounted on the retraction pipe 61.
In addition, a pressure balance member 7 is connected to the mixing tank 1, the pressure balance member 7 includes a balance pipe 71 connected to the mixing tank 1, a fourth control valve 72 is connected to the balance pipe 71, and the balance pipe 71 is communicated with the top end of the passive cavity 152. The part of the material guiding pipe 19 located in the power cavity 151 is connected with a base pipe 25, the inner wall of the base pipe 25 is rectangular, and the horizontal width of the inner wall of the base pipe 25 is larger than the inner diameter of the material guiding pipe 19. Two closing plates 22 are arranged on the inner wall of the base pipe 25 in a relatively sliding manner, a one-way valve 26 is arranged at the position, above the closing plates 22, of the material guide pipe 19, and a driving assembly 8 for driving the closing plates 22 to slide is arranged on the material guide pipe 19.
When the mixed liquid is added into the liquid storage area 12 for the first time, the fourth control valve 72 is opened to ensure that the balance pipe 71 is communicated, the mixed liquid is injected into the liquid storage cavity 17 through the feed pipe 18, and the material guide pipe 19 is sealed by the sealing plate 22; when the mixed liquid in the liquid storage cavity 17 reaches a specified amount, the fourth control valve 72 is closed, the balance pipe 71 is closed, and a sealed cavity is formed between the piston plate 21 and the liquid level of the mixed liquid; then, the fifth control valve 24 is opened, the driving assembly 8 drives the closing plate 22 to slide, and the material guide pipes 19 are communicated; liquid is added into the power cavity 151 through the fluid pipe 23, at this time, the piston plate 21 moves downwards due to the pressure, the mixed liquid in the passive cavity 152 is pressed into the material guiding pipe 19 and enters the lowest mixing cavity 15, and the first feeding into the mixing cavity 15 is completed. When the subsequent feeding to the passive cavity 152 is finished, the balance pipe 71 is opened, the third control valve 62 is opened, the receiving and releasing pipe 61 is communicated, the liquid storage cavity 17 is pumped out through the receiving and releasing pipe 61 while the feeding is finished, the piston plate 21 is pulled up, after the feeding is finished to a proper amount, the third control valve 62 is used, the driving assembly 8 drives the sealing plate 22 to slide, the liquid is fed into the power cavity 151 through the liquid pipe 23, and the mixed liquid is continuously fed into the mixing cavity 15 at the lowest part for multiple times.
As shown in fig. 3 and 4, the driving assembly 8 in this embodiment includes a base block 81, a driving gear 82, a driving toothed plate 83, a reversing gear 84, a reversing toothed plate 85 and an elastic pull rope 86, the base block 81 is fixedly connected to the inner wall of the tube of the base tube 25, the base blocks 81 are arranged in two opposite directions, sliding grooves 811 are formed on the side walls of the two opposite sides of the base blocks 81, and the closing plate 22 is arranged on the corresponding sliding groove 811 in a sliding manner. A driving cavity 812 communicated with the sliding groove 811 is formed in the base block 81, one end, extending into the driving cavity 812, of the sealing plate 22 is fixedly connected with a linked toothed plate 87, the driving gear 82 is rotatably arranged on the cavity wall of the driving cavity 812 and is positioned below the linked toothed plate 87, the bottom wall of the driving gear 82 is meshed with the top end of the linked toothed plate 87, the cavity wall of the driving cavity 812 is also rotatably connected with a matching gear 88, and the matching gear 88 is meshed with the reversing gear 84; the driving toothed plate 83 is arranged on the wall of the driving cavity 812 in a sliding manner along the sliding direction of the closing plate 22, and the top wall of the driving toothed plate 83 is meshed with the bottom end of the reversing gear 84; and a positioning spring 831 is fixedly connected between one end of the driving gear 82 facing the closing plate 22 and the wall of the driving cavity 812. One end of the driving toothed plate 83, which is far away from the positioning spring 831, is fixedly connected with a reversing plate 89, a through groove 191 communicated with the driving cavity 812 is formed in the material guide pipe 19, the reversing plate 89 extends out of the driving cavity 812 through the through groove 191 and is connected with the groove wall of the through groove 191 in a sliding manner, and the reversing plate 89 is in sealing fit with the groove wall of the through groove 191.
Fixedly connected with base plate 841 is located on the lateral wall of the blending tank body 1 in power cavity 151, the shape of base plate 841 is set for as required, it is connected with switching-over runner 891 to rotate on the vertical lateral wall of base plate 841, switching-over pinion rack 85 slides along vertical direction and sets up on base plate 841 lateral wall and is located switching-over runner 891 below, fixedly connected with switching-over rope 842 between one end that switching-over plate 89 stretches out the passage 19 and switching-over pinion rack 85 top, switching-over rope 842 and one side lateral wall butt that switching-over runner 891 deviates from the passage 19. The reversing gear 84 is rotatably arranged on the vertical side wall of the base plate 841 and is meshed with the reversing toothed plate 85; the reversing gear 84 is coaxially connected with a retracting wheel 843, meanwhile, a coil spring 845 is connected between the rotating shaft of the retracting roller and the side wall of the reversing gear 84, one end of an elastic pull rope 86 is fixedly connected with the retracting wheel 843, and the other end of the elastic pull rope 86 bypasses the retracting wheel 843 and is fixedly connected with the top wall of the piston plate 21.
Under the elastic force of the positioning spring 831, the driving toothed plate 83 is positioned at a specified position, and the closing plate 22 stably closes the material guide pipe 19; when the piston plate 21 moves downwards, the elastic pull rope 86 drives the retraction wheel 843 to rotate, and the coil spring 845 is stretched; the reversing gear 84 rotates along with the retracting wheel 843, then the matching gear 88 is meshed with the reversing toothed plate 85, the reversing gear 84 is meshed with the matching gear 88, the reversing gear 84 is meshed with the linkage toothed plate 87, the closing plate 22 rotates, the closing plate 22 opens the material guide pipe 19, and the positioning spring 831 is stretched. Then the piston plate 21 is moved downwards continuously, at this time, the retraction wheel 843 does not rotate any more, and the elastic pull rope 86 is elastically deformed, so that the piston plate 21 can smoothly press the mixed liquid into the material guide pipe 19. After the piston plate 21 moves upwards, the elastic pulling rope 86 is firstly restored to the natural state, then under the elastic force action of the coil spring 845 and the positioning spring 831, the elastic pulling rope 86 is wound on the retracting wheel 843 again, the toothed plate 83 is driven to return to the original position, and the closing plate 22 closes the material guide pipe 19 again.
As shown in fig. 5 and fig. 6, the feed delivery assembly 3 comprises a feed delivery pipe 31, a connecting pipe 32 and a feed delivery pipe 33, the feed delivery pipe 31 is fixedly connected to the partition plate 14, the top end of the feed delivery pipe 31 extends into the bottom wall of the mixing chamber 15 in the direction, the bottom end of the feed delivery pipe 31 extends into the bottom end of the mixing chamber 15 below, and the feed delivery pipe 31 is hermetically connected with the partition plate 14; the connecting pipe 32 is fixedly connected to the outer wall of the mixing tank body 1 and is connected with the power pump 34, and two end walls of the connecting pipe 32 far away from the power pump 34 extend into the mixing cavity 15 in the middle. Furthermore, one end of the connecting pipe 32 extending into the mixing chamber 15 is connected to one feed pipe 31 in the mixing chamber 15, and the other end of the connecting pipe 32 extending into the mixing chamber 15 is connected to the other feed pipe 31 in the mixing chamber 15. Two parts of the connecting pipe 32 extending into the mixing cavity 15 are connected with a feeding pipe 33 and a second control valve 35, the feeding pipe 33 is provided with a first control valve 36, and the two feeding pipes 33 are positioned between the two second control valves 35.
The second control valve 35 adjacent to the uppermost mixing chamber 15 is closed, the first control valve 36 on the feeding pipe 33 adjacent to the lowermost mixing chamber 15 is closed, the power pump 34 is started, and the mixed liquid in the lowermost mixing chamber 15 is introduced into the middle mixing chamber 15 through the feeding pipe 19, the connecting pipe 32, and the feeding pipe 33 adjacent to the uppermost mixing chamber 15. The second control valve 35 adjacent to the lowermost mixing chamber 15 is closed, the first control valve 36 on the feed pipe 33 adjacent to the uppermost mixing chamber 15 is closed, the power pump 34 is started, and the mixed liquid in the intermediate mixing chamber 15 is introduced into the uppermost mixing chamber 15 through the feed pipe 33 adjacent to the lowermost mixing chamber 15, the connecting pipe 32, and the material guide pipe 19.
As shown in fig. 5, the mixing device 4 in this embodiment includes a heater 41 mounted on the mixing tank 1 and a rotary base shaft 42 rotatably connected between the partition plates 14, the rotary base shaft 42 is provided with a stirring blade 43, the top wall of the mixing tank 1 is provided with a motor 44, and the motor 44 is fixedly connected with the top end of the rotary base shaft 42. Meanwhile, the discharging assembly 5 in this embodiment comprises a discharging pipe 51 connected to the mixing tank body 1 and a discharging pump 52 connected to the discharging pipe 51, and the discharging pipe 51 is communicated with the uppermost mixing chamber 15. The motor 44 and the heater 41 are started, the mixed liquid can be mixed in the mixing chamber 15, and finally the discharge pump 52 is started, so that the mixed liquid in the uppermost mixing chamber 15 can be output.
The working principle of the equipment for the preparation method of the silicon carbide thin-walled tube is as follows: the mixed solution is divided into two parts, wherein one part is mixed with the mixed powder in advance. Adding one portion of the mixture to one of the passive chambers 152 and another portion of the mixture to the other passive chamber 152; the balance pipe 71 is closed, liquid is added into the power cavity 151 through the liquid pipe 23, the piston plate 21 moves downwards, the material guide pipe 19 is opened by the closing plate 22, and then the two mixed liquids are sent into the mixing cavity 15 at the lowest part; the mixed liquid is mixed for the first time in the mixing chamber 15 at the lowest position, at the same time, the balance pipe 71 is opened, new mixed liquid is added into the passive chamber 152, the liquid in the power chamber 151 is pumped out through the receiving pipe 61, the piston plate 21 moves upwards, and the closing plate 22 closes the material guiding pipe 19 until the mixed liquid is added to a proper amount. After the mixed liquid is mixed in the mixing cavity 15 at the lowest part, the mixed liquid is conveyed to the mixing cavity 15 at the middle part through the material conveying component 3 to be mixed continuously, and at the moment, the mixed liquid in the power cavity 151 is added into the mixing cavity 15 at the lowest part continuously; so that the mixed liquid is continuously mixed in the three mixing chambers 15 for the same total mixing time, and finally the discharge pump 52 is started, so that the mixed liquid in the uppermost mixing chamber 15 can be conveyed to the next mechanism.
Comparative example
Comparative example 1
Comparative example 1 differs from example 1 in that: no new base methyl CMC-BL is added.
Comparative example 2
Comparative example 2 differs from example 1 in that: the amount of the new parison methyl CMC-BL is 2.5wt% of the silicon carbide.
Comparative example 3
Comparative example 3 differs from example 1 in that: the new blank methyl CMC-BL is replaced by the same amount of sodium carboxymethyl cellulose.
Comparative example 4
Comparative example 4 differs from example 1 in that: the new green methyl CMC-BL was replaced with an equal amount of ceramic reinforcing agent FG-560.
Performance detection
For the products of examples 1-12 and comparative examples 1-4:
and (3) detecting the density of the silicon carbide thin-walled tube by using a silicon carbide ceramic densimeter and a drainage method.
And detecting the outer diameter of the silicon carbide thin-walled tube by using an infrared diameter measuring instrument, detecting and calculating the wall thickness difference of the detected silicon carbide thin-walled tube by using the inner diameter of the silicon carbide thin-walled tube by using a caliper, wherein the wall thickness difference is the difference between the maximum wall thickness and the minimum wall thickness. Wherein, the wall thickness of the silicon carbide thin-wall pipe in the embodiment is 0.1-0.3mm.
And detecting the out-of-roundness of the silicon carbide thin-wall pipe by using an infrared diameter gauge, wherein the out-of-roundness is the difference between the maximum pipe outer diameter and the minimum pipe outer diameter of the silicon carbide thin-wall pipe.
And on a marble platform, detecting the straightness of the silicon carbide thin-walled tube by using a feeler gauge.
The performance test data are shown in Table 3
TABLE 3 table for examining the properties of examples 1 to 10 and comparative examples 1 to 4
According to the detection results of the embodiments 1 to 3, the silicon carbide thin-wall tube still has a good shape and is convenient to assemble under the condition that the wall thickness is 0.1 to 0.3mm, and the silicon carbide thin-wall tube in the embodiment has proper density and good wear resistance and corrosion resistance. The silicon carbide nanotubes of example 1 performed best. And the detection results of the embodiment 4 and the embodiment 5 and the detection results of the comparative examples 1 to 4 show that the selection of the novel green methyl CMC-BL and the control of the content of the novel green methyl CMC-BL both have influence on the performance of the silicon carbide thin-wall tube and may be caused by the matching of the performance of the novel green methyl CMC-BL and the growth process of silicon carbide grains.
From the results of the tests in examples 7 and 8, it is understood that the control of the molding conditions has no influence on the density of the thin silicon carbide pipe and has a certain influence on the form of the thin silicon carbide pipe, but the influence is not so great.
From the detection results of the embodiments 9 to 12, it can be known that the influence of the sintering process parameters on the density and the form of the silicon carbide thin-walled tube is large, and particularly, the influence of the process parameters in the temperature rising stage on the silicon carbide thin-walled tube is large. Probably because the high temperature sintering has a relatively large influence on the growth of the silicon carbide crystal grains.
The above embodiments are preferred embodiments of the present application, and the protection scope of the present application is not limited by the above embodiments, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (10)
1. A silicon carbide thin-wall tube is characterized in that: the raw materials comprise the following components: silicon carbide; the plasticizer accounts for 10-13wt% of the silicon carbide; the new parison methyl CMC-BL, the consumption of said new parison methyl CMC-BL is 0.2-2wt% of the silicon carbide; a lubricant, wherein the amount of the lubricant is 1-4wt% of the silicon carbide; the using amount of the dispersing agent is 10-20wt% of the silicon carbide; and the amount of the water is 20-30wt% of the silicon carbide.
2. The silicon carbide thin-walled tube of claim 1, wherein: the plasticizer is hydroxypropyl methyl cellulose, the lubricant is at least one of glycerol and oleic acid, and the dispersant is polyethylene glycol.
3. The method for preparing the silicon carbide thin-walled tube according to claim 1 or 2, wherein: the method comprises the following steps:
mixing: mixing silicon carbide, a plasticizer and the novel blank with methyl CMC-BL to obtain mixed powder; uniformly mixing water, a lubricant and a dispersant to obtain a mixed solution, uniformly mixing the mixed solution and the mixed powder, carrying out vacuum mixing, and sealing and ageing to obtain aged mud;
molding: extruding and molding the aged pug, and drying to obtain a thin-wall tube blank;
and (3) high-temperature sintering: and sintering the thin-walled tube blank to obtain the silicon carbide thin-walled tube.
4. The method for preparing the silicon carbide thin-walled tube according to claim 3, wherein: in the molding step, after the aged pug is extruded and molded, air floatation support is carried out, and the air pressure is 0.1-0.6Mpa; and drying by microwave at 50-80 deg.C.
5. The method for preparing the silicon carbide thin-walled tube according to claim 3, wherein the method comprises the following steps: the high-temperature sintering operation comprises the following steps:
degreasing: heating to 600-1100 deg.C under vacuum micro-negative pressure, heating at a rate of 1-3 deg.C/min, and maintaining for 10-60min;
and (3) heating: heating to 1100-1900 deg.c at a rate of 3-10 deg.c/min for 20-30min;
and (3) sintering: filling argon to 10-50KPa, heating to 1900-2100 deg.C at a rate of 1-5 deg.C/min, and maintaining for 10-55min;
and (3) cooling: cooling to 1500-1800 ℃, preserving heat for 30-60min, and finally cooling to room temperature to obtain the silicon carbide thin-wall tube.
6. An apparatus for use in the method of manufacturing a silicon carbide thin-walled tube according to claim 3, characterized in that: the equipment is used for mixing the mixed liquid and the mixed powder; the equipment comprises a mixing tank body (1), and is characterized in that: the inner wall of the mixing tank body (1) is provided with a partition plate (11), the mixing tank body (1) is divided into a liquid storage area (12) and a mixing area (13) by the partition plate (11) from bottom to top, the inner wall of the mixing tank body (1) positioned in the mixing area (13) is provided with a partition plate (14), and the mixing area (13) is divided into mixing cavities (15) which are arranged from bottom to top by the partition plate (14); a sub-baffle (16) is arranged between the inner wall of the liquid storage area (12) of the mixing tank body (1) and the partition plate (11), and the sub-baffle (16) divides the liquid storage area (12) into at least two liquid storage cavities (17); a feeding pipe (18) communicated with each liquid storage cavity (17) is arranged on the mixing tank body (1), a material guide pipe (19) is arranged between each liquid storage cavity (17) and the mixing cavity (15) adjacent to the liquid storage area (12), and a material guide assembly (2) is arranged in each liquid storage cavity (17); a material conveying assembly (3) for conveying materials in the lower mixing cavity (15) to the upper mixing cavity (15) is arranged between the adjacent mixing cavities (15), and a mixing device (4) is arranged in each mixing cavity (15); the mixing tank body (1) is provided with a discharge assembly (5) communicated with the mixing cavity (15) at the uppermost part.
7. An apparatus for the preparation of silicon carbide thin walled tubes according to claim 6, wherein: the material guide assembly (2) comprises a piston plate (21) and a closing plate (22), the piston plate (21) is arranged on the wall of the liquid storage cavity (17) in a sliding mode along the vertical direction, the vertical side wall of the piston plate (21) is connected with the wall of the mixing cavity (15) in a sealing mode, the mixing cavity (15) is divided into a power cavity (151) located above and a driven cavity (152) located below by the piston plate (21), the bottom end of the material guide pipe (19) penetrates through the piston plate (21) and is connected with the piston plate (21) in a sliding mode, and the outer wall of the material guide pipe (19) is connected with the piston plate (21) in a sealing mode; a fluid pipe (23) communicated with the power cavity (151) is connected to the mixing tank body (1), and the fluid pipe (23) is connected with a retraction assembly (6) for the fluid to enter and exit; the mixing tank body (1) is connected with a pressure balancing piece (7) communicated with the passive cavity (152); the sealing plate (22) is arranged on the inner wall of the material guiding pipe (19) in a sliding mode, a one-way valve (26) is arranged on the material guiding pipe (19), the sealing plate (22) is located between the one-way valve (26) and the piston plate (21), and a driving assembly (8) used for driving the sealing plate (22) to slide is arranged on the material guiding pipe (19).
8. The apparatus for preparing the silicon carbide thin-walled tube according to claim 7, wherein: the driving assembly (8) comprises a base block (81), a driving gear (82), a driving toothed plate (83), a reversing gear (84), a reversing toothed plate (85) and an elastic pull rope (86), wherein the base block (81) is arranged on the side wall of the material guide pipe (19) relatively, one end, deviating from the side wall of the material guide pipe (19) connected with the base block (81), is provided with a sliding groove (811), the closing plate (22) is arranged on the groove wall of the sliding groove (811) in a sliding manner, a driving cavity (812) is arranged in the base block (81) and is communicated with the sliding groove (811), one end, extending into the driving cavity (812), of the closing plate (22) is provided with a linkage toothed plate (87), the driving gear (82) is arranged on the cavity wall of the driving cavity (812) in a rotating manner, the driving gear (82) is meshed with the linkage toothed plate (87), a matching gear (88) is further connected to the cavity wall of the driving cavity (812) in a rotating manner, and the matching gear (88) is meshed with the linkage gear; the driving toothed plate (83) is arranged on the wall of the driving cavity (812) in a sliding mode, and the driving toothed plate (83) is meshed with the matching gear (88); a positioning spring (831) is arranged between the driving gear (82) and the wall of the driving cavity (812); a reversing plate (89) is arranged on the driving toothed plate (83), and the reversing plate (89) extends out of the material guide pipe (19) and is connected with the material guide pipe (19) in a sliding manner; a base plate (841) is arranged on the cavity wall of the power cavity (151), a reversing rotating wheel (891) is rotatably connected to the base plate (841), the reversing toothed plate (85) is arranged on the base plate (841) in a sliding manner along the vertical direction, a reversing rope (842) is connected between one end of the reversing plate (89) extending out of the material guide pipe (19) and the top end of the reversing toothed plate (85), and the reversing rope (842) is abutted to the reversing rotating wheel (891); the reversing gear (84) is rotatably arranged on the base plate (841), and the reversing gear (84) is meshed with the reversing toothed plate (85); the reversing gear (84) is coaxially connected with a retracting wheel (843), a coil spring (845) is arranged between the retracting wheel (843) and the side wall of the reversing gear (84), one end of an elastic pull rope (86) is fixedly connected with the retracting wheel, and the other end of the elastic pull rope (86) bypasses the retracting wheel (843) and the piston plate (21) to be fixedly connected.
9. The apparatus for preparing the silicon carbide thin-walled tube according to claim 7, wherein: the material conveying assembly (3) comprises material conveying pipes (31), connecting pipes (32) and material conveying pipes (33), the material conveying pipes (31) are arranged between the adjacent mixing cavities (15), and the material conveying pipes (31) penetrate through the partition plates (14) and are in sealing connection with the partition plates (14); connecting pipe (32) are connected between double-phase adjacent conveying pipeline (31) bottom and top, it has two and connects to walk material pipe (33) on connecting pipe (32), be connected with power pump (34) on connecting pipe (32), power pump (34) are located two walk between material pipe (33), it is provided with first control valve (36) on material pipe (33) to walk, be provided with two second control valve (35) on connecting pipe (32), power pump (34) with it all is located two to walk material pipe (33) between second control valve (35).
10. The apparatus for preparing the silicon carbide thin-walled tube according to claim 7, wherein: mixing arrangement (4) is including installing heater (41) on the blending tank body (1) are connected with rotating the rotation base shaft (42) between division board (14), install stirring piece (43) on rotating base shaft (42), motor (44) are installed to the blending tank body (1) roof, motor (44) with the top fixed connection who rotates base shaft (42).
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| CN202211033485.5A CN115321984A (en) | 2022-08-26 | 2022-08-26 | Silicon carbide thin-wall pipe and manufacturing method and equipment thereof |
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| CN202211033485.5A CN115321984A (en) | 2022-08-26 | 2022-08-26 | Silicon carbide thin-wall pipe and manufacturing method and equipment thereof |
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Application publication date: 20221111 |