CN104908143A - Preparation method for laser sintering 3D (three-dimensional) printing rapid prototyping alumina powder - Google Patents
Preparation method for laser sintering 3D (three-dimensional) printing rapid prototyping alumina powder Download PDFInfo
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- CN104908143A CN104908143A CN201510284342.5A CN201510284342A CN104908143A CN 104908143 A CN104908143 A CN 104908143A CN 201510284342 A CN201510284342 A CN 201510284342A CN 104908143 A CN104908143 A CN 104908143A
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- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
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- 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
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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Abstract
The invention discloses a preparation method for laser sintering 3D (three-dimensional) printing rapid prototyping alumina powder. The preparation method is characterized in that distearoyl isopropoxy aluminate is adopted to pretreat alumina powder in the solvent of acetic ether, so that pretreated alumina powder is obtained; 84 to 90 percent of the pretreat alumina powder, 2 to 5 percent of thermoplastic phenolic resin, 2 to 5 percent of perchlorovinyl resin and 1.0 to 6 percent of carbon powder are then added into a grinding machine according to percentage by weight, the grinding machine is started to carry out grinding for 5 minutes at the rotational speed of 320 rotations per minute, 2 to 8 percent of acetone is then added, the sum of all the components is 100 percent, the grinding machine carries out grinding again for 60 to 80 minutes at the rotational speed of 320 rotations per minute, and after drying, the laser sintering 3D printing rapid prototyping alumina powder is obtained. The material can be directly prototyped under laser sintering, the prototyping precision is high, high temperature can be resisted, moreover, the preparation process is simple, conditions are easy to control, the production cost is low, and the material is easy to produce industrially.
Description
Technical field
The present invention relates to a kind of preparation method for laser sintering rapid forming dusty material, belong to the Material Field of rapid shaping, particularly a kind of laser sintered 3D prints the preparations and applicatio of rapid shaping alumina powder.
Background technology
3D prints (3D printing), is a kind of based on mathematical model file, use flow-like, Powdered, silk (rod) shape etc. curable, bond, alloying material, carried out the technology of constructed object by the mode of successively solidifying, bonding, fusing.The field such as Making mold, industrial design of being everlasting is used to modeling, after gradually for the direct manufacture of some products, had the parts using this technology to print.This technology is at jewelry, footwear, industrial design, building, engineering and construction (AEC), automobile, and Aero-Space, dentistry and medical industries, education, GIS-Geographic Information System, civil engineering, gun and other field are applied all to some extent.3D printing technique appears at the mid-90 in 20th century, is actually the up-to-date rapid molding device of technology such as utilizing photocuring and ply of paper to fold.It is substantially identical with common print operation principle, and printer, built with liquid or powder etc. " printed material ", after being connected, is stacked up " printed material " by conputer controlled from level to level with computer, finally the blueprint on computer is become in kind.This printing technique is called 3D three-dimensional printing technology.Traditional manufacture generally needs to cut raw material or hole, and namely subtracts material manufacture, can be mass-produced; It is by material stacking bonding, fusion from level to level that 3D prints, and namely increases material manufacture; Quick individual character manufacturing can be realized, the shape that traditional manufacture cannot complete can be produced.
3D printed material is the important substance basis of 3D printing technique development, and to a certain extent, can the development of material decide 3D and print have and apply widely.At present, 3D printed material mainly comprises engineering plastics, photosensitive resin, rubber type of material, metal material and ceramic material etc.The excellent specific properties such as ceramic material has high strength, high rigidity, high temperature resistant, low-density, chemical stability are good, corrosion-resistant, have a wide range of applications in industries such as Aero-Space, automobile, biologies.But because the feature that ceramic material is hard and crisp makes it shape especially difficulty, particularly complicated ceramic component need be shaped by mould, and Mould Machining cost is high, the construction cycle is long, is difficult to the demand meeting product continuous renewal.The ceramic powders that 3D prints is the mixture that ceramic powder and certain adhesive powder form.Because the fusing point of adhesive powder is low, just ceramic powders is bondd together adhesive powder fusing time laser sintered, need ceramic to put in temperature controlling stove, carry out post processing at a higher temperature.The proportioning of ceramic powders and adhesive powder, mixability can have influence on the performance of ceramic component.Binding agent ratio is higher, and sintering is than being easier to, but in last handling process, parts shrinkage ratio is comparatively large, can affect the dimensional accuracy of parts.Otherwise adhesive consumption is few, be then not easy sintering.
The laser sintered a kind of method belonging to increasing material and manufacture.This technique is also take laser instrument as energy source, by laser beam, the powder of plastics, wax, pottery, metal or its compound is sintered equably on processing plane.The powder of uniform spreading last layer very thin (submillimeter level) is as raw material on the table, and laser beam under control of the computer, is scanned by the 2-D data of point aspect with certain speed and energy density by scanner.After laser beam flying, the powder of relevant position just sinters certain thickness entity lamella into, and the place do not scanned still keeps loose Powdered.After this one deck is scanned, need subsequently to scan lower one deck.First cut layer thickness and layering thickness according to object and reduce workbench, powder is paved by paving powder cylinder again, can start the scanning of new one deck.So repeatedly, until scanned structure at all levels.Remove excessive powder, and through post processing, can product be obtained.
In existing moulding material field, because SLS (selective laser sintering) rapid shaping technique has the advantages such as raw material sources various and structure time that is part is shorter, therefore have in rapid shaping field and apply more widely.But major part is organic material and composite, a kind of nylon powder material for laser sintering and moulding goods is disclosed in Chinese invention patent CN1379061A, by the improvement of chemical synthesis and technique, the surface of nylon powder material is processed, obtain sintering character excellent, moulded products intensity is high, the product of good toughness, simplify the preparation technology of laser sintered nylon material, reduce cost; A kind of laser sintered 3D manufacturing technology stone plastic composite powder end and preparation method thereof is disclosed in Chinese invention patent CN103881371.
Aluminium oxide ceramics is a kind of with aluminium oxide (Al
2o
3) be the ceramic material of main body, for thick film integrated circuit.Aluminium oxide ceramics has good conductibility, mechanical strength and heat-resisting quantity.Aluminium oxide ceramics is a kind of broad-spectrum pottery, as ceramic bearing, ceramic seal and water valve plate, make melten glass to replace platinum crucible, utilize its light transmission and sodium vapor lamp pipe can be used as by alkaline-resisting metal protection, can be used as ic substrate and high-frequency insulation material etc. in the electronics industry.
The present invention is by carrying out face coat modification to aluminium oxide powder material, and by the surface of high molecular adhesive coating to Ultrafine Aluminium Oxide Particle, the coating rear oxidation aluminium powder material obtained directly can adopt laser sintering rapid forming.This powder can reach micron and submicron order, and adhesive coating is even, and adhesive consumption is few, and bond effect is good, and intensity is large, and post processing is simple, and the dusty material of uniform particle diameter.This material can be shaped precision, abnormal shape, complicated parts quickly and easily, does not need to spray bonding agent, greatly simplifies and just do program.Not only intensity is high for institute's product that obtains, and also makes the realization be molded on 3D rapidform machine of thin-walled micro parts become possibility; In addition, the method that this patent provides is simple, and cost is low.
Summary of the invention
Order of the present invention is to provide the preparation method that a kind of laser sintered 3D prints rapid shaping alumina powder, and rapid shaping powder does not need to spray binding agent can Direct Laser scanning moulding;
Object of the present invention is achieved through the following technical solutions.
Laser sintered 3D prints a preparation method for rapid shaping alumina powder, and it is characterized in that, the method has following processing step:
(1) alumina powder pretreatment: in the reactor, adds by mass percentage, ethyl acetate: 48% ~ 56%, distearyl acyl-oxygen isopropyl Aluminate: 10% ~ 16%, stirring and dissolving, then add alumina powder: 31% ~ 40%, each component sum is absolutely, strong stirring, in 40 ± 2 DEG C of isothermal reaction 6 ~ 8 h, after cooling, filtration, filtrate recycling, washing, drying, obtains pretreatment alumina powder;
(2) laser sintered 3D prints the preparation of rapid shaping alumina powder: in grinder, add by mass percentage, process alumina powder: 84% ~ 90%, novolac resin: 2% ~ 5%, superchlorinated polyvinyl chloride resin: 2% ~ 5%, carbon dust: 1.0% ~ 6%, open grinder rotating speed at 320 revs/min, grinding 5min, add acetone again: 2% ~ 8%, each component sum is absolutely, grinder rotating speed is at 320 revs/min, grind 60 ~ 80min again, dry, obtain laser sintered 3D and print rapid shaping alumina powder, the particle diameter that the laser sintered 3D obtained prints rapid shaping alumina powder is in the scope of 0.5 ~ 2.0 μm.
The particle diameter of alumina powder described is in step (1) within the scope of 0.5 ~ 1.5 μm;
Novolac resin described in step (2) and the mass ratio of superchlorinated polyvinyl chloride resin are optimum between 1:0.8 ~ 1.5.
Alumina powder described in step (2) and the mass ratio of carbon dust are optimum between 1:0.02 ~ 0.05.
Particle size test method of the present invention is the granularity equivalent diameter size adopting laser particle analyzer to record.
Another object of the present invention is to provide laser sintered 3D and prints the application shaping on 3D printer of rapid shaping aluminium oxide powder material, feature is: laser sintered 3D is printed rapid shaping aluminium oxide powder material and join in the confession powder cylinder of selective laser sintering and moulding machine, dusty material to be layered on processing plane and to be heated to processing temperature by paving powder roller equably, laser instrument sends laser, the switch of computer controlled laser and the angle of scanner, the two-dimentional sheet-shaped of laser beam according to correspondence on processing plane is scanned, after laser beam is inswept, workbench moves down a thickness, repave powder, laser beam flying, so repeatedly, obtain laser sintered, the mode that wherein laser beam scans on processing plane is subregion scanning, and laser power is 30 ~ 50W, and sweep speed is 1500mm/s, and sweep span is 0.1 ~ 0.15mm, and lift height is 0.10 ~ 0.2mm, preheat temperature: 50 DEG C, and processing temperature is 120 ~ 130 DEG C.
Compared with the prior art, tool has the following advantages and beneficial effect in the present invention:
(1) the laser sintered 3D that the present invention obtains prints rapid shaping aluminium oxide powder material, not needing to spray binding agent can straight forming under laser sintered condition, owing to adding the carbon dust with light absorptive and reproducibility in preparation process, in forming process, the absorption efficiency of material for laser light improves, and does not also produce splash.
(2) the laser sintered 3D that the present invention obtains prints rapid shaping aluminium oxide powder material, and particle can reach submicron order even nanoscale, has meso-position radius grain little, the feature that particle size distribution is narrow, stable in properties; Can manufacture thin-walled model or small parts by this rapid shaping dusty material, producing product, to have surface gloss high, and intensity is good, precision high.
(3) the laser sintered 3D that the present invention obtains prints rapid shaping aluminium oxide powder material, has preparation technology simple, and condition is easy to control, and production cost is low, is easy to suitability for industrialized production, has again the advantage such as low-carbon environment-friendly and economize energy.
(4) the laser sintered 3D that the present invention obtains prints rapid shaping aluminium oxide powder material, can effective rapid shaping on laser sintered 3D printer, and shaping precision is high.
Detailed description of the invention
Embodiment 1
(1) alumina powder pretreatment: in the reactor, add respectively, ethyl acetate: 58 mL, distearyl acyl-oxygen isopropyl Aluminate: 13g, stirring and dissolving, then add alumina powder: 35g, strong stirring, in 40 ± 2 DEG C of isothermal reaction 7 h, after cooling, filtration, washing, drying, obtain pretreatment alumina powder;
(2) laser sintered 3D prints the preparation of rapid shaping alumina powder: in grinder, add respectively, process alumina powder: 87g, novolac resin: 3g, superchlorinated polyvinyl chloride resin: 3g, carbon dust: 4g, open grinder rotating speed at 320 revs/min, grinding 5min, then add acetone: 4 mL, grinder rotating speed is at 320 revs/min, grind 70min again, drying, obtains laser sintered 3D and prints rapid shaping alumina powder, and the particle diameter that the laser sintered 3D obtained prints rapid shaping alumina powder is in the scope of 0.5 ~ 2.0 μm.
Embodiment 2
(1) alumina powder pretreatment: in the reactor, add respectively, ethyl acetate: 62 mL, distearyl acyl-oxygen isopropyl Aluminate: 10g, stirring and dissolving, then add alumina powder: 34g, strong stirring, in 40 ± 2 DEG C of isothermal reaction 6 h, after cooling, filtration, washing, drying, obtain pretreatment alumina powder;
(2) laser sintered 3D prints the preparation of rapid shaping alumina powder: in grinder, add respectively, process alumina powder: 85g, novolac resin: 5g, superchlorinated polyvinyl chloride resin: 5g, carbon dust: 2g, open grinder rotating speed at 320 revs/min, grinding 5min, then add acetone: 10 mL, grinder rotating speed is at 320 revs/min, grind 60min again, drying, obtains laser sintered 3D and prints rapid shaping alumina powder, and the particle diameter that the laser sintered 3D obtained prints rapid shaping alumina powder is in the scope of 0.5 ~ 2.0 μm.
Embodiment 3
(1) alumina powder pretreatment: in the reactor, add respectively, ethyl acetate: 53 mL, distearyl acyl-oxygen isopropyl Aluminate: 12g, stirring and dissolving, then add alumina powder: 40g, strong stirring, in 40 ± 2 DEG C of isothermal reaction 8h, after cooling, filtration, washing, drying, obtain pretreatment alumina powder;
(2) laser sintered 3D prints the preparation of rapid shaping alumina powder: in grinder, add respectively, process alumina powder: 90g, novolac resin: 2g, superchlorinated polyvinyl chloride resin: 2g, carbon dust: 3g, open grinder rotating speed at 320 revs/min, grinding 5min, then add acetone: 7mL, grinder rotating speed is at 320 revs/min, grind 65min again, drying, obtains laser sintered 3D and prints rapid shaping alumina powder, and the particle diameter that the laser sintered 3D obtained prints rapid shaping alumina powder is in the scope of 0.5 ~ 2.0 μm.
Embodiment 4
(1) alumina powder pretreatment: in the reactor, add respectively, ethyl acetate: 60 mL, distearyl acyl-oxygen isopropyl Aluminate: 15g, stirring and dissolving, then add alumina powder: 32g, strong stirring, in 40 ± 2 DEG C of isothermal reaction 7.5 h, after cooling, filtration, washing, drying, obtain pretreatment alumina powder;
(2) laser sintered 3D prints the preparation of rapid shaping alumina powder: in grinder, add respectively, process alumina powder: 86g, novolac resin: 3g, superchlorinated polyvinyl chloride resin: 2g, carbon dust: 1g, open grinder rotating speed at 320 revs/min, grinding 5min, then add acetone: 9mL, grinder rotating speed is at 320 revs/min, grind 75min again, drying, obtains laser sintered 3D and prints rapid shaping alumina powder, and the particle diameter that the laser sintered 3D obtained prints rapid shaping alumina powder is in the scope of 0.5 ~ 2.0 μm.
Embodiment 5
(1) alumina powder pretreatment: in the reactor, add respectively, ethyl acetate: 55 mL, distearyl acyl-oxygen isopropyl Aluminate: 16g, stirring and dissolving, then add alumina powder: 34g, strong stirring, in 40 ± 2 DEG C of isothermal reaction 6.5 h, after cooling, filtration, washing, drying, obtain pretreatment alumina powder;
(2) laser sintered 3D prints the preparation of rapid shaping alumina powder: in grinder, add respectively, process alumina powder: 88g, novolac resin: 2g, superchlorinated polyvinyl chloride resin: 3g, carbon dust: 3g, open grinder rotating speed at 320 revs/min, grinding 5min, then add acetone: 5 mL, grinder rotating speed is at 320 revs/min, grind 80min again, drying, obtains laser sintered 3D and prints rapid shaping alumina powder, and the particle diameter that the laser sintered 3D obtained prints rapid shaping alumina powder is in the scope of 0.5 ~ 2.0 μm.
Embodiment 6
(1) alumina powder pretreatment: in the reactor, add respectively, ethyl acetate: 61 mL, distearyl acyl-oxygen isopropyl Aluminate: 14g, stirring and dissolving, then add alumina powder: 31g, strong stirring, in 40 ± 2 DEG C of isothermal reaction 7 h, after cooling, filtration, washing, drying, obtain pretreatment alumina powder;
(2) laser sintered 3D prints the preparation of rapid shaping alumina powder: in grinder, add respectively, process alumina powder: 84g, novolac resin: 2g, superchlorinated polyvinyl chloride resin: 2g, carbon dust: 5g, open grinder rotating speed at 320 revs/min, grinding 5min, then add acetone: 8mL, grinder rotating speed is at 320 revs/min, grind 70min again, drying, obtains laser sintered 3D and prints rapid shaping alumina powder, and the particle diameter that the laser sintered 3D obtained prints rapid shaping alumina powder is in the scope of 0.5 ~ 2.0 μm.
Using method: laser sintered 3D is printed rapid shaping aluminium oxide powder material and join in the confession powder cylinder of selective laser sintering and moulding machine, dusty material to be layered on processing plane and to be heated to processing temperature by paving powder roller equably, laser instrument sends laser, the switch of computer controlled laser and the angle of scanner, the two-dimentional sheet-shaped of laser beam according to correspondence on processing plane is scanned, after laser beam is inswept, workbench moves down a thickness, repave powder, laser beam flying, so repeatedly, laser sintered is obtained; The mode that wherein laser beam scans on processing plane is subregion scanning, and laser power is 30 ~ 50W, and sweep speed is 1500mm/s, and sweep span is 0.1 ~ 0.15mm, and lift height is 0.10 ~ 0.2mm, preheat temperature: 50 DEG C, and processing temperature is 120 ~ 130 DEG C.
Claims (5)
1. laser sintered 3D prints a preparation method for rapid shaping alumina powder, and it is characterized in that, the method has following processing step:
(1) alumina powder pretreatment: in the reactor, adds by mass percentage, ethyl acetate: 48% ~ 56%, distearyl acyl-oxygen isopropyl Aluminate: 10% ~ 16%, stirring and dissolving, then add alumina powder: 31% ~ 40%, each component sum is absolutely, strong stirring, in 40 ± 2 DEG C of isothermal reaction 6 ~ 8 h, after cooling, filtration, filtrate recycling, washing, drying, obtains pretreatment alumina powder;
(2) laser sintered 3D prints the preparation of rapid shaping alumina powder: in grinder, add by mass percentage, process alumina powder: 84% ~ 90%, novolac resin: 2% ~ 5%, superchlorinated polyvinyl chloride resin: 2% ~ 5%, carbon dust: 1.0% ~ 6%, open grinder rotating speed at 320 revs/min, grinding 5min, add acetone again: 2% ~ 8%, each component sum is absolutely, grinder rotating speed is at 320 revs/min, grind 60 ~ 80min again, dry, obtain laser sintered 3D and print rapid shaping alumina powder, the particle diameter that the laser sintered 3D obtained prints rapid shaping alumina powder is in the scope of 0.5 ~ 2.0 μm.
2. a kind of laser sintered 3D according to claim 1 prints the preparation method of rapid shaping alumina powder, and it is characterized in that, the particle diameter of the alumina powder described in step (1) is within the scope of 0.5 ~ 1.5 μm.
3. a kind of laser sintered 3D according to claim 1 prints the preparation method of rapid shaping alumina powder, it is characterized in that, the mass ratio of the novolac resin described in step (2) and superchlorinated polyvinyl chloride resin is optimum between 1:0.8 ~ 1.5.
4. a kind of laser sintered 3D according to claim 1 prints the preparation method of rapid shaping alumina powder, it is characterized in that, the mass ratio of the alumina powder described in step (2) and carbon dust is optimum between 1:0.02 ~ 0.05.
5. a kind of laser sintered 3D according to claim 1 prints the laser sintered 3D printing rapid shaping alumina powder prepared by the preparation method of rapid shaping alumina powder, it is characterized in that, the condition of molding that described laser sintered 3D prints rapid shaping alumina powder is: laser power is 30 ~ 50W, sweep speed is 1500mm/s, sweep span is 0.1 ~ 0.15mm, lift height is 0.10 ~ 0.2mm, preheat temperature: 50 DEG C, and processing temperature is 120 ~ 130 DEG C.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105215260A (en) * | 2015-09-21 | 2016-01-06 | 济南大学 | A kind of for the low precoated sand preparation method that gets angry of laser sintered 3D printing |
| CN105669208A (en) * | 2016-03-07 | 2016-06-15 | 武汉理工大学 | Phenolic resin coated ceramic powder for laser 3D printing and preparation method thereof |
| CN106986579A (en) * | 2017-03-28 | 2017-07-28 | 常州大学 | A kind of preparation method of lower shrinkage 3D printing material |
| CN108372301A (en) * | 2017-01-04 | 2018-08-07 | 中国航空制造技术研究院 | A kind of powder of selective laser fusing elaborates device and method |
| CN110901063A (en) * | 2019-12-18 | 2020-03-24 | 杭州德迪智能科技有限公司 | Targeted induction and directional energy composite three-dimensional forming device and method |
| CN115322524A (en) * | 2022-08-25 | 2022-11-11 | 江苏集萃先进高分子材料研究所有限公司 | Polyester elastomer powder for selective laser sintering and preparation method thereof |
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| JPH02107670A (en) * | 1988-10-17 | 1990-04-19 | Murata Mfg Co Ltd | Packaging resin, electronic part and laser-marking of electronic part |
| KR101070505B1 (en) * | 2006-05-12 | 2011-10-05 | 덴끼 가가꾸 고교 가부시키가이샤 | Ceramic powder and applications thereof |
| CN103980608A (en) * | 2014-04-30 | 2014-08-13 | 中国科学院化学研究所 | Polypropylene nanocomposite material capable of being used for 3D printing, and preparation method and application thereof |
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| JPH02107670A (en) * | 1988-10-17 | 1990-04-19 | Murata Mfg Co Ltd | Packaging resin, electronic part and laser-marking of electronic part |
| KR101070505B1 (en) * | 2006-05-12 | 2011-10-05 | 덴끼 가가꾸 고교 가부시키가이샤 | Ceramic powder and applications thereof |
| CN103980608A (en) * | 2014-04-30 | 2014-08-13 | 中国科学院化学研究所 | Polypropylene nanocomposite material capable of being used for 3D printing, and preparation method and application thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105215260A (en) * | 2015-09-21 | 2016-01-06 | 济南大学 | A kind of for the low precoated sand preparation method that gets angry of laser sintered 3D printing |
| CN105669208A (en) * | 2016-03-07 | 2016-06-15 | 武汉理工大学 | Phenolic resin coated ceramic powder for laser 3D printing and preparation method thereof |
| CN108372301A (en) * | 2017-01-04 | 2018-08-07 | 中国航空制造技术研究院 | A kind of powder of selective laser fusing elaborates device and method |
| CN106986579A (en) * | 2017-03-28 | 2017-07-28 | 常州大学 | A kind of preparation method of lower shrinkage 3D printing material |
| CN110901063A (en) * | 2019-12-18 | 2020-03-24 | 杭州德迪智能科技有限公司 | Targeted induction and directional energy composite three-dimensional forming device and method |
| CN115322524A (en) * | 2022-08-25 | 2022-11-11 | 江苏集萃先进高分子材料研究所有限公司 | Polyester elastomer powder for selective laser sintering and preparation method thereof |
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