CN116332636B - Special material for carbon-doped bismuth oxide powder injection molding and method for preparing bismuth oxide ceramic by laser irradiation sintering - Google Patents
Special material for carbon-doped bismuth oxide powder injection molding and method for preparing bismuth oxide ceramic by laser irradiation sintering Download PDFInfo
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- 229910000416 bismuth oxide Inorganic materials 0.000 title claims abstract description 62
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000000843 powder Substances 0.000 title claims abstract description 53
- 238000005245 sintering Methods 0.000 title claims abstract description 33
- 239000000463 material Substances 0.000 title claims abstract description 29
- 238000001746 injection moulding Methods 0.000 title claims abstract description 26
- 239000011224 oxide ceramic Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 229920000642 polymer Polymers 0.000 claims abstract description 14
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 13
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 13
- 229910021392 nanocarbon Inorganic materials 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000006229 carbon black Substances 0.000 claims abstract description 11
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 239000002243 precursor Substances 0.000 claims abstract description 11
- 239000004642 Polyimide Substances 0.000 claims abstract description 10
- 239000004793 Polystyrene Substances 0.000 claims abstract description 10
- 239000002131 composite material Substances 0.000 claims abstract description 10
- 229920001721 polyimide Polymers 0.000 claims abstract description 10
- 229920002223 polystyrene Polymers 0.000 claims abstract description 10
- 230000004044 response Effects 0.000 claims abstract description 10
- 238000002347 injection Methods 0.000 claims description 15
- 239000007924 injection Substances 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 9
- 239000002048 multi walled nanotube Substances 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 13
- 230000008569 process Effects 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000001000 micrograph Methods 0.000 description 5
- 238000005452 bending Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229930040373 Paraformaldehyde Natural products 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- -1 polyoxymethylene Polymers 0.000 description 2
- 229920006324 polyoxymethylene Polymers 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012778 molding material Substances 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
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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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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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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- C04B35/64—Burning or sintering processes
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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
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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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
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5284—Hollow fibers, e.g. nanotubes
- C04B2235/5288—Carbon nanotubes
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- C04B2235/54—Particle size related information
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- C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
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Abstract
The invention belongs to the technical field of powder injection molding and laser irradiation sintering, and particularly relates to a special material for carbon-doped bismuth oxide powder injection molding and a method for preparing bismuth oxide ceramics by laser irradiation sintering. The special material for carbon doped bismuth oxide powder injection molding comprises the following components in parts by mass: 100-200 parts of bismuth oxide powder, 1-5 parts of carbon nano tube, 2-6 parts of nano carbon black, 20-30 parts of polystyrene and 5-10 parts of polyimide. The laser irradiation sintering method comprises the following steps: mixing the raw materials in an internal mixer according to a certain proportion, crushing, extruding, granulating, injection molding, and then sintering at a high temperature under the condition of laser irradiation. According to the invention, the carbon nano tube and the nano carbon black are used as the composite laser response catalyst, the polystyrene and the polyimide are used as the polymer precursor carbon source, and the laser irradiation sintering technology is used for carrying out in-situ sintering on the special material, so that the carbon doping efficiency and the doping uniformity are improved, and the problem of low compactness of the finished product is solved.
Description
Technical Field
The invention belongs to the technical field of powder injection molding and laser irradiation sintering, and particularly relates to a special material for carbon-doped bismuth oxide powder injection molding and a method for preparing bismuth oxide ceramics by laser irradiation sintering.
Background
The powder injection molding combines the powder metallurgy technology and the plastic injection molding technology, takes a mixed system of metal (or metal oxide) powder and polymer as a feed, gives fluidity to the mixed system by means of high temperature and high pressure of an injection molding machine, injects the mixed system in a viscous state into a mold cavity, and cools to obtain a green body. And obtaining a final finished product through degreasing, high-temperature sintering and other processes. The finished product of powder injection molding has the characteristics of precise structure, simple process and the like, and is widely applied to the manufacture of precise parts in the fields of consumer electronics, automobiles and the like.
In order to improve the application performance of metal (or metal oxide) finished products in fields of photocatalysis and the like, the most common method is to dope carbon elements in metal (or metal oxide) powder, but due to the long time, usually several hours, required by the traditional high-temperature sintering process, the doped carbon substances are oxidized or agglomerated at high temperature for a long time, so that the density of the final finished products is lower and the carbon doping amount is difficult to control. The laser irradiation technology is to irradiate the sample with laser of certain wavelength and energy, and the sample absorbs great amount of laser energy instantaneously to reach high temperature to realize compact sintering of the sample.
Disclosure of Invention
In order to solve the problems, the invention provides a special material for injection molding of carbon-doped bismuth oxide powder and a method for preparing bismuth oxide ceramics by laser irradiation sintering, which creatively uses a polymer easy to form carbon by laser as a precursor carbon source, introduces a laser response type carbon catalyst, and completes the process of doping carbon element in a high-density finished product while performing laser irradiation sintering.
The special material for carbon doped bismuth oxide powder injection molding consists of bismuth oxide powder, a laser response composite catalyst and a polymer precursor carbon source; the laser response composite catalyst is formed by mixing carbon nanotubes and nano carbon black; the polymer precursor carbon source is formed by mixing polystyrene and polyimide.
Wherein, each raw material component is as follows according to the mass portion: 100-200 parts of bismuth oxide powder, 1-5 parts of carbon nano tube, 2-6 parts of nano carbon black, 20-30 parts of polystyrene and 5-10 parts of polyimide.
Preferably, the bismuth oxide powder has a particle size in the range of 200-500nm.
Preferably, the carbon nanotubes are multi-walled carbon nanotubes with a diameter of 10-20nm and a length of 10-20 μm; the particle size range of the nano carbon black is 10-100nm.
Preferably, both polystyrene and polyimide are thermoplastic polymers without any surface modification treatment.
The method for preparing bismuth oxide ceramic by laser irradiation sintering comprises the following steps:
(1) Mixing bismuth oxide powder, a laser response composite catalyst and a polymer precursor carbon source in proportion, and mixing for 20min at 60 ℃ by using a high-speed mixer to finish primary mixing;
(2) Putting the materials mixed in the step (1) into an internal mixer, uniformly mixing, preparing a feed, crushing, extruding and granulating by using a single screw extruder, and preparing the special material for injection molding of the carbon-doped bismuth oxide powder;
(3) The special powder injection material is injected into an injection blank and is placed under laser irradiation, the bismuth oxide powder and the laser response composite catalyst absorb a large amount of laser energy and reach instantaneous high temperature, so that the polymer precursor carbon source is carbonized in situ, and the bismuth oxide powder is sintered and densified into porcelain at high temperature.
Preferably, the temperature of the internal mixer in the step (2) is set to 200 ℃, the rotating speed is 60r/min, and the time is 15 minutes; the temperature of the single screw extruder was set to: 160 ℃,170 ℃,180 ℃,185 ℃,190 ℃,190 ℃ and the rotating speed is 100rpm.
Preferably, the laser in step (3) is a near infrared laser beam with a wavelength of 1064nm. The laser irradiation parameters were set as follows: the laser power is 60-120W, and the scanning speed is 100-500mm/s.
The beneficial effects of the invention are as follows:
compared with the traditional carbon material direct addition and high-temperature sintering process, the laser response composite catalyst is introduced to improve the absorption degree of the special powder injection molding material on near infrared laser, and meanwhile, the laser irradiation sintering process is used to absorb a large amount of laser energy at the moment of laser irradiation, the instantaneous temperature can reach 1500 ℃, the carbonization product of the polymer instantly completes the doping process, agglomeration is not easy, the growth of crystal grains is not limited, and the compactness of the bismuth oxide ceramic finished product is improved.
2, the invention solves the problem of low compactness of bismuth oxide powder in the sintering process, introduces the polymer which is easy to form carbon by laser as a polymer precursor carbon source, generates nano carbon substances on the surface of bismuth oxide in the laser irradiation process, and has the functions of doping modification, wherein the nano carbon substances are uniformly dispersed and easily enter bismuth oxide lattices.
Description of the drawings:
FIG. 1 is a scanning electron microscope image of bismuth oxide powder of example 1;
FIG. 2 is a scanning electron microscope image of bismuth oxide ceramic prepared in example 1;
FIG. 3 is a scanning electron microscope image of bismuth oxide ceramic prepared in example 2;
FIG. 4 is a scanning electron microscope image of bismuth oxide ceramic prepared in example 3;
fig. 5 is a scanning electron microscope image of the bismuth oxide ceramic prepared in comparative example 4.
Detailed Description
Example 1
The special material for carbon doped bismuth oxide powder injection molding and the preparation of bismuth oxide ceramics by laser irradiation sintering thereof comprise the following steps:
(1) The special material for the injection molding of the carbon-doped bismuth oxide powder is prepared from the following raw materials in parts by mass: 120 parts of bismuth oxide powder (particle size 300 nm), 2 parts of carbon nano-tube, 3 parts of nano-carbon black, 20 parts of polystyrene and 6 parts of polyimide.
(2) And (3) placing the prepared raw materials into a high-speed mixer to mix for 20min at 60 ℃ to finish primary mixing.
(3) The mixed raw materials are uniformly mixed in an internal mixer, the temperature is set to 200 ℃, the rotating speed is 60r/min, and the time is 15 minutes. After crushing, uniformly granulating by using a single-screw extruder, wherein the temperature of each zone of the single-screw extruder is set as follows: 160 ℃,170 ℃,180 ℃,185 ℃,190 ℃, and the rotating speed of 100rpm, and granulating to prepare the special powder injection material.
(4) The powder injection special material is injected into an injection blank and is placed under laser irradiation, the laser energy is 110W, the laser speed scanning rate is 220mm/s, the bismuth oxide ceramic is prepared by instantaneous sintering and molding, and SEM pictures are shown in figure 2.
Example 2
The special material for carbon doped bismuth oxide powder injection molding and the preparation of bismuth oxide ceramics by laser irradiation sintering thereof comprise the following steps:
(1) The special material for the injection molding of the carbon-doped bismuth oxide powder is prepared from the following raw materials in parts by mass: 120 parts of bismuth oxide powder (with the particle size of 400 nm), 4 parts of carbon nano-tubes, 6 parts of nano-carbon black, 20 parts of polystyrene and 6 parts of polyimide.
(2) And (3) placing the prepared raw materials into a high-speed mixer to mix for 20min at 60 ℃ to finish primary mixing.
(3) The mixed raw materials are uniformly mixed in an internal mixer, the temperature is set to 200 ℃, the rotating speed is 60r/min, and the time is 15 minutes. After crushing, uniformly granulating by using a single-screw extruder, wherein the temperature of each zone of the single-screw extruder is set as follows: 160 ℃,170 ℃,180 ℃,185 ℃,190 ℃, and the rotating speed of 100rpm, and granulating to prepare the special powder injection material.
(4) The powder injection special material is injected into an injection blank and is placed under laser irradiation, the laser energy is 85W, the laser speed scanning rate is 300mm/s, the bismuth oxide ceramic is prepared by instantaneous sintering and molding, and SEM pictures are shown in figure 3.
Example 3
The special material for carbon doped bismuth oxide powder injection molding and the preparation of bismuth oxide ceramics by laser irradiation sintering thereof comprise the following steps:
(1) The special material for the injection molding of the carbon-doped bismuth oxide powder is prepared from the following raw materials in parts by mass: 120 parts of bismuth oxide powder (particle size 500 nm), 4 parts of carbon nano-tube, 2 parts of nano-carbon black, 15 parts of polystyrene and 8 parts of polyimide.
(2) And (3) placing the prepared raw materials into a high-speed mixer to mix for 20min at 60 ℃ to finish primary mixing.
(3) The mixed raw materials are uniformly mixed in an internal mixer, the temperature is set to 200 ℃, the rotating speed is 60r/min, and the time is 15 minutes. After crushing, uniformly granulating by using a single-screw extruder, wherein the temperature of each zone of the single-screw extruder is set as follows: 160 ℃,170 ℃,180 ℃,185 ℃,190 ℃, and the rotating speed of 100rpm, and granulating to prepare the special powder injection material.
(4) The powder injection special material is injected into an injection blank and is placed under laser irradiation, the laser energy is 70W, the laser speed scanning rate is 450mm/s, the bismuth oxide ceramic is prepared by instantaneous sintering and molding, and SEM pictures are shown in figure 4.
Comparative example 1
Compared with the embodiment 1, the sintering mode is changed into high-temperature sintering, the sintering temperature is 1200 ℃, and the sintering time is 120min.
Comparative example 2
In comparison with example 1, the laser energy was adjusted to 30W, and the remaining conditions were unchanged. Due to the fact that the laser energy is too low, the generated sintering temperature is low, the density of the finished product is reduced, the carbon doping amount is reduced, and the bending strength of the finished product is low.
Comparative example 3
The laser scanning rate was adjusted to 800mm/s as compared with example 1, with the remaining conditions unchanged. Because the scanning speed of the laser is too high, the residence time of the laser is reduced, and enough heat cannot be generated, so that the density of the finished product is reduced, the carbon doping amount is reduced, and the bending strength of the finished product is lower.
Comparative example 4
The particle size of the bismuth oxide powder was adjusted to 10 μm as compared with example 1, and the remaining conditions were unchanged. As the particle size of the bismuth oxide powder increases, the energy generated by the laser irradiation is insufficient to densify the bond between the bismuth oxide powder, and the final product is still in a loose powder form, the SEM picture of which is shown in fig. 5.
Comparative example 5
Compared with example 1, the carbon source of the polymer precursor was adjusted to 20 parts of polyethylene glycol, 6 parts of polyoxymethylene, and the remaining conditions were unchanged. Because polyethylene glycol and polyoxymethylene mainly undergo degradation reaction under laser irradiation, carbon formation is difficult, so that the carbon doping amount in the finished bismuth oxide product is low, and the bending strength is reduced.
Comparative example 6
In comparison with example 1, the laser-responsive composite catalyst was adjusted so that only 2 parts of carbon nanotubes were added, and the remaining conditions were unchanged. Because the light-heat conversion efficiency of a single carbon nano tube under laser irradiation is limited, enough heat cannot be generated, and the density of the finished bismuth oxide product is low, which is manifested by reduced bending strength.
TABLE 1 partial Properties of bismuth oxide ceramics prepared in examples 1-3 and comparative examples 1-6
Claims (3)
1. The method for preparing bismuth oxide ceramic by laser irradiation sintering is characterized in that the bismuth oxide ceramic is prepared by adopting a special material for injection molding of carbon-doped bismuth oxide powder, wherein the special material for injection molding of the powder consists of bismuth oxide powder, a laser response composite catalyst and a polymer precursor carbon source; the particle size of the bismuth oxide powder ranges from 200 nm to 500nm; the laser response composite catalyst is formed by mixing carbon nanotubes and nano carbon black; the polymer precursor carbon source is formed by mixing polystyrene and polyimide; the special material for powder injection molding comprises the following raw material components in parts by mass: 100-200 parts of bismuth oxide powder, 1-5 parts of carbon nano tube, 2-6 parts of nano carbon black, 20-30 parts of polystyrene and 5-10 parts of polyimide; the method comprises the following steps:
(1) Mixing bismuth oxide powder, a laser response composite catalyst and a polymer precursor carbon source in proportion, and mixing for 20min at 60 ℃ by using a high-speed mixer to finish primary mixing;
(2) Putting the materials mixed in the step (1) into an internal mixer, uniformly mixing, preparing a feed, crushing, extruding and granulating by using a single screw extruder, and preparing the special material for injection molding of the carbon-doped bismuth oxide powder;
(3) Injecting the special powder injection material into an injection blank, and placing the injection blank under laser irradiation to sinter and compact the injection blank into bismuth oxide ceramic; the laser is a near infrared laser beam with the wavelength of 1064nm; the laser irradiation parameters were set as follows: the laser power is 60-120W, and the scanning speed is 100-500mm/s.
2. The method for preparing bismuth oxide ceramic by laser irradiation sintering according to claim 1, wherein the carbon nanotubes are multi-wall carbon nanotubes with a diameter of 10-20nm and a length of 10-20 μm; the particle size of the nano carbon black is 10-100nm.
3. The method for preparing bismuth oxide ceramic by laser irradiation sintering according to claim 1, wherein the temperature of the internal mixer in the step (2) is set to 200 ℃, the rotating speed is 60r/min, and the time is 15 minutes; the temperature of the single screw extruder was set to: 160 ℃,170 ℃,180 ℃,185 ℃,190 ℃,190 ℃ and the rotating speed is 100rpm.
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| JP2002121067A (en) * | 2000-10-10 | 2002-04-23 | Kyocera Corp | Zinc oxide-based sintered compact and method of producing the same |
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| JP2010095396A (en) * | 2008-10-15 | 2010-04-30 | Tokan Material Technology Co Ltd | Bismuth oxide-based additive for laser marking and production method of the same |
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