CN104788102A - Preparation method for nano-silicon nitride powder for laser sintering 3D printing technology - Google Patents
Preparation method for nano-silicon nitride powder for laser sintering 3D printing technology Download PDFInfo
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Abstract
The invention discloses a preparation method for a nano-silicon nitride powder for the laser sintering 3D printing technology. The preparation method is characterized by comprising the following steps: firstly, using gamma-glycidoxypropyl trimethoxysilane for the pretreatment of nano-silicon nitride powder in an ethanol solvent to obtain pretreated nano-silicon nitride powder; then, adding the following components by mass percentage into a grinding machine to obtain a mixture I: 84%-90% of pretreated nano-silicon nitride powder, 3%-8% of epoxy resin and 0.4%-1.0% of pyromellitic dianhydride, starting the grinding machine, grinding the mixture I at a revolution speed of 300 rpm for 5 min, and then adding 5%-10% of acetone to obtain a mixture II, turning on the grinding machine, grinding the mixture II at a revolution speed of 300 rpm for 30-40 min, and drying the grinded mixture II to obtain the nano-silicon nitride powder for laser sintering 3D printing technology. The nano-silicon nitride powder for the laser sintering 3D printing technology can be molded directly under laser sintering, is simple in preparation process, low in production cost, and easy to realize industrial production, and the condition is easy to control.
Description
Technical field
The present invention relates to a kind of preparation method printing manufacturing technology powdered molding material for laser sintered 3D, belong to the Material Field of rapid shaping, particularly a kind of preparations and applicatio of laser sintered 3D printing technique nano-silicon nitride powder.
Background technology
The laser sintered a kind of method belonging to increasing material and manufacture.This technique is also take laser apparatus as energy source, by laser beam, the powder of plastics, wax, pottery, metal or its mixture 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 scanning device.After laser beam flying, the powder of corresponding 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 worktable, 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 aftertreatment, can product be obtained.
Although the domestic research for new pattern laser sintering for quick formation material is at present a lot, but be mostly confined to the moulding process to existing material, part performance studies, and the precision of institute's steps of manufacturing blanks, intensity and weather resistance etc. also far away can not the requirements of content with funtion part, also do not produce special rapid prototyping material manufacturers.This situation not only affects the quality of rapid laser sintering molding material or molded article, but also is unfavorable for the Industry Promotion of laser sintering rapid prototyping technology.Exploitation easily shaping, that intensity is high, pollution-free, cost is low type material has become the problem that laser sintering rapid prototyping technology primarily solves.
3D prints (3D printing), is a kind of based on digital 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 component using this technology to print.This technology is at jewelry, footwear, industrial design, building, engineering and construction (AEC), automobile, and aerospace, dentistry and medical industries, education, geographical information system(GIS), civil engineering work, 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 principle of work, 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 starting 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.
In existing formed 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 materials and matrix material, a kind of nylon powder material for laser sintering and moulding goods is disclosed in Chinese invention patent CN1379061A, by the improvement of chemosynthesis 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.
The chemical resistance of silicon nitride ceramics is good, intensity is high, hardness is high, and wear resisting property is good, frictional coefficient is little, high temperature resistant, and the advantages such as density is low, all have application prospect as structured material or functional materials, receive increasing concern in recent years.Silicon nitride ceramics obtains a wide range of applications at industrial circles such as oil, chemical industry, microelectronics, space flight, aviation, papermaking, laser, automobile, mining industry and nuclear power.The preparation method of current silicon nitride ceramics mainly contains: powder compression sintering process, sol-gel method and reaction sintering etc., when adopting aforesaid method to prepare silicon nitride member, need the mould first according to the shape preparation of component with respective shapes, if the shape of component slightly changes, just need again to prepare mould or need to carry out mechanical workout to sample, thus increase preparation cost.Because the restriction aforesaid method being subject to mould is commonly used to the component preparing simple shape.
The present invention is by carrying out top coat modification to silicon nitride powder powder material, and by high molecular adhesive coating to superfine silicon nitride ceramic powder material surface, after the coating obtained, silicon nitride ceramic powder material directly can adopt laser sintering rapid forming.This powder can reach nano level, and the powdered material of uniform particle diameter.This material can be shaped precision, abnormal shape, complicated parts quickly and easily, does not need to spray caking 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 a kind of preparation method of laser sintered 3D printing technique nano-silicon nitride 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.
A preparation method for laser sintered 3D printing technique nano-silicon nitride powder, is characterised in that the method has following processing step:
(1) nano-silicon nitride powder pre-treatment: in the reactor, add by mass percentage, ethanol: 40% ~ 50%, γ-glycidyl ether oxygen propyl trimethoxy silicane: 18% ~ 26%, stirs, then adds nano-si 3 n 4 ceramics powder: 30% ~ 35%, each component sum is absolutely, be placed in 60 ± 5 DEG C of constant temperature, strong stirring, back flow reaction 2 ~ 4 h, filtering separation, filtrate liquid reclaims, by washing with alcohol, drying, grinding, obtains pre-treatment nano-silicon nitride powder;
(2) preparation of laser sintered 3D printing technique nano-silicon nitride powder: in shredder, add by mass percentage, pre-treatment nano-silicon nitride powder: 84% ~ 90%, epoxy resin: 3% ~ 8%, pyromellitic dianhydride: 0.4% ~ 1.0%, open shredder rotating speed at 300 revs/min, grinding 5min, add acetone again: 5% ~ 10%, each component sum is absolutely, open shredder rotating speed at 300 revs/min, grinding 30 ~ 40min, dry, obtain laser sintered 3D printing technique nano-silicon nitride powder, the particle diameter of the laser sintered 3D printing technique nano-silicon nitride powder obtained is in the scope of 0.1 ~ 0.5 μm.
The particle diameter of nano-si 3 n 4 ceramics powder described is in step (1) within the scope of 0.1 ~ 0.4 μm;
Filtrate after separation described is in step (1) reclaimed, and adds a certain amount of γ-glycidyl ether oxygen propyl trimethoxy silicane and reuses.
The solid epoxy of oxirane value between 0.2 ~ 04 of the epoxy resin described in step (2).
Epoxy resin described in step (2) and the mass ratio of pyromellitic dianhydride are optimum between 1:0.08 ~ 0.12.
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 the application shaping on 3D printer of laser sintered 3D printing technique nano-silicon nitride powdered material, feature is: joined by laser sintered 3D printing technique nano-silicon nitride powdered material in the confession powder cylinder of selective laser sintering and moulding machine, powdered material to be layered on processing plane and to be heated to processing temperature by paving powder roller equably, laser apparatus sends laser, the switch of computer controlled laser and the angle of scanning device, the two-dimentional sheet-shaped of laser beam according to correspondence on processing plane is scanned, after laser beam is inswept, worktable 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 20 ~ 40W, and sweep velocity is 1500mm/s, and sweep span is 0.1 ~ 0.15mm, and lift height is 0.10 ~ 0.2mm, preheating 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 printing technique nano-silicon nitride powdered material of the present invention's acquisition, not needing to spray binding agent can straight forming under laser sintered condition.
(2) the laser sintered 3D printing technique nano-silicon nitride powdered material of the present invention's acquisition, particle can reach nano level, has meso-position radius grain little, the feature that particle size distribution is narrow, stable in properties; Can manufacture thin-walled model or small component by this rapid shaping powdered material, producing product, to have surface gloss high, and intensity is good, precision high.
(3) the laser sintered 3D printing technique nano-silicon nitride powdered material of the present invention's acquisition, 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 save energy.
(4) the laser sintered 3D printing technique nano-silicon nitride powdered material that obtains of the present invention, can effective rapid shaping on laser sintered 3D printer, and shaping precision is high.
Embodiment
Embodiment 1
(1) nano-silicon nitride powder pre-treatment: in the reactor, add respectively, ethanol: 57 mL, γ-glycidyl ether oxygen propyl trimethoxy silicane: 22 mL, stir, then add nano-si 3 n 4 ceramics powder: 32g, be placed in 60 DEG C of constant temperature, strong stirring, back flow reaction 3 h, filtering separation, filtrate liquid reclaims, by washing with alcohol, dry, grinding, obtains pre-treatment nano-silicon nitride powder;
(2) preparation of laser sintered 3D printing technique nano-silicon nitride powder: in shredder, add respectively, pre-treatment nano-silicon nitride powder: 87g, epoxy resin: 5g, pyromellitic dianhydride: 0.5g, open shredder rotating speed at 300 revs/min, grinding 5min, add acetone again: 10 mL, open shredder rotating speed at 300 revs/min, grinding 35min, dry, obtain laser sintered 3D printing technique nano-silicon nitride powder, the particle diameter of the laser sintered 3D printing technique nano-silicon nitride powder obtained is in the scope of 0.1 ~ 0.5 μm.
Embodiment 2
(1) nano-silicon nitride powder pre-treatment: in the reactor, add respectively, ethanol: 63 mL, γ-glycidyl ether oxygen propyl trimethoxy silicane: 19 mL, stir, then add nano-si 3 n 4 ceramics powder: 30g, be placed in 55 DEG C of constant temperature, strong stirring, back flow reaction 2h, filtering separation, filtrate liquid reclaims, by washing with alcohol, dry, grinding, obtains pre-treatment nano-silicon nitride powder;
(2) preparation of laser sintered 3D printing technique nano-silicon nitride powder: in shredder, add respectively, pre-treatment nano-silicon nitride powder: 84g, epoxy resin: 8g, pyromellitic dianhydride: 1g, open shredder rotating speed at 300 revs/min, grinding 5min, add acetone again: 9 mL, open shredder rotating speed at 300 revs/min, grinding 30min, dry, obtain laser sintered 3D printing technique nano-silicon nitride powder, the particle diameter of the laser sintered 3D printing technique nano-silicon nitride powder obtained is in the scope of 0.1 ~ 0.5 μm.
Embodiment 3
(1) nano-silicon nitride powder pre-treatment: in the reactor, add respectively, ethanol: 51 mL, γ-glycidyl ether oxygen propyl trimethoxy silicane: 24 mL, stir, then add nano-si 3 n 4 ceramics powder: 35g, be placed in 65 DEG C of constant temperature, strong stirring, back flow reaction 4 h, filtering separation, filtrate liquid reclaims, by washing with alcohol, dry, grinding, obtains pre-treatment nano-silicon nitride powder;
(2) preparation of laser sintered 3D printing technique nano-silicon nitride powder: in shredder, add respectively, pre-treatment nano-silicon nitride powder: 90g, epoxy resin: 4g, pyromellitic dianhydride: 0.4g, open shredder rotating speed at 300 revs/min, grinding 5min, add acetone again: 7 mL, open shredder rotating speed at 300 revs/min, grinding 40min, dry, obtain laser sintered 3D printing technique nano-silicon nitride powder, the particle diameter of the laser sintered 3D printing technique nano-silicon nitride powder obtained is in the scope of 0.1 ~ 0.5 μm.
Embodiment 4
(1) nano-silicon nitride powder pre-treatment: in the reactor, add respectively, ethanol: 53 mL, γ-glycidyl ether oxygen propyl trimethoxy silicane: 23 mL, stir, then add nano-si 3 n 4 ceramics powder: 34g, be placed in 62 DEG C of constant temperature, strong stirring, back flow reaction 3.5 h, filtering separation, filtrate liquid reclaims, by washing with alcohol, dry, grinding, obtains pre-treatment nano-silicon nitride powder;
(2) preparation of laser sintered 3D printing technique nano-silicon nitride powder: in shredder, add respectively, pre-treatment nano-silicon nitride powder: 85g, epoxy resin: 7g, pyromellitic dianhydride: 0.6g, open shredder rotating speed at 300 revs/min, grinding 5min, add acetone again: 9mL, open shredder rotating speed at 300 revs/min, grinding 32min, dry, obtain laser sintered 3D printing technique nano-silicon nitride powder, the particle diameter of the laser sintered 3D printing technique nano-silicon nitride powder obtained is in the scope of 0.1 ~ 0.5 μm.
Embodiment 5
(1) nano-silicon nitride powder pre-treatment: in the reactor, add respectively, ethanol: 62 mL, γ-glycidyl ether oxygen propyl trimethoxy silicane: 17 mL, stir, then add nano-si 3 n 4 ceramics powder: 33g, be placed in 57 DEG C of constant temperature, strong stirring, back flow reaction 2.5 h, filtering separation, filtrate liquid reclaims, by washing with alcohol, dry, grinding, obtains pre-treatment nano-silicon nitride powder;
(2) preparation of laser sintered 3D printing technique nano-silicon nitride powder: in shredder, add respectively, pre-treatment nano-silicon nitride powder: 84g, epoxy resin: 6g, pyromellitic dianhydride: 1g, open shredder rotating speed at 300 revs/min, grinding 5min, add acetone again: 13 mL, open shredder rotating speed at 300 revs/min, grinding 38min, dry, obtain laser sintered 3D printing technique nano-silicon nitride powder, the particle diameter of the laser sintered 3D printing technique nano-silicon nitride powder obtained is in the scope of 0.1 ~ 0.5 μm.
Embodiment 6
(1) nano-silicon nitride powder pre-treatment: in the reactor, add respectively, ethanol: 60 mL, γ-glycidyl ether oxygen propyl trimethoxy silicane: 21 mL, stir, then add nano-si 3 n 4 ceramics powder: 31g, be placed in 60 DEG C of constant temperature, strong stirring, back flow reaction 4 h, filtering separation, filtrate liquid reclaims, by washing with alcohol, dry, grinding, obtains pre-treatment nano-silicon nitride powder;
(2) preparation of laser sintered 3D printing technique nano-silicon nitride powder: in shredder, add respectively, pre-treatment nano-silicon nitride powder: 88g, epoxy resin: 6g, pyromellitic dianhydride: 0.7g, open shredder rotating speed at 300 revs/min, grinding 5min, add acetone again: 6 mL, open shredder rotating speed at 300 revs/min, grinding 40min, dry, obtain laser sintered 3D printing technique nano-silicon nitride powder, the particle diameter of the laser sintered 3D printing technique nano-silicon nitride powder obtained is in the scope of 0.1 ~ 0.5 μm.
Using method: laser sintered 3D printing technique nano-silicon nitride powdered material is joined in the confession powder cylinder of selective laser sintering and moulding machine, powdered material to be layered on processing plane and to be heated to processing temperature by paving powder roller equably, laser apparatus sends laser, the switch of computer controlled laser and the angle of scanning device, the two-dimentional sheet-shaped of laser beam according to correspondence on processing plane is scanned, after laser beam is inswept, worktable 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 20 ~ 40W, and sweep velocity is 1500mm/s, and sweep span is 0.1 ~ 0.15mm, and lift height is 0.10 ~ 0.2mm, preheating temperature: 50 DEG C, and processing temperature is 120 ~ 130 DEG C.It is high that the product obtained has shaping precision.
Claims (6)
1. a preparation method for laser sintered 3D printing technique nano-silicon nitride powder, it is characterized in that, the method has following processing step:
(1) nano-silicon nitride powder pre-treatment: in the reactor, add by mass percentage, ethanol: 40% ~ 50%, γ-glycidyl ether oxygen propyl trimethoxy silicane: 18% ~ 26%, stirs, then adds nano-si 3 n 4 ceramics powder: 30% ~ 35%, each component sum is absolutely, be placed in 60 ± 5 DEG C of constant temperature, strong stirring, back flow reaction 2 ~ 4 h, filtering separation, filtrate liquid reclaims, by washing with alcohol, drying, grinding, obtains pre-treatment nano-silicon nitride powder;
(2) preparation of laser sintered 3D printing technique nano-silicon nitride powder: in shredder, add by mass percentage, pre-treatment nano-silicon nitride powder: 84% ~ 90%, epoxy resin: 3% ~ 8%, pyromellitic dianhydride: 0.4% ~ 1.0%, open shredder rotating speed at 300 revs/min, grinding 5min, add acetone again: 5% ~ 10%, each component sum is absolutely, open shredder rotating speed at 300 revs/min, grinding 30 ~ 40min, dry, obtain laser sintered 3D printing technique nano-silicon nitride powder, the particle diameter of the laser sintered 3D printing technique nano-silicon nitride powder obtained is in the scope of 0.1 ~ 0.5 μm.
2. the preparation method of a kind of laser sintered 3D printing technique nano-silicon nitride powder according to claim 1, it is characterized in that, the particle diameter of the nano-si 3 n 4 ceramics powder described in step (1) is within the scope of 0.1 ~ 0.4 μm.
3. the preparation method of a kind of laser sintered 3D printing technique nano-silicon nitride powder according to claim 1, it is characterized in that, filtrate after separation described in step (1) is reclaimed, and adds a certain amount of γ-glycidyl ether oxygen propyl trimethoxy silicane and reuses.
4. the preparation method of a kind of laser sintered 3D printing technique nano-silicon nitride powder according to claim 1, is characterized in that, the solid epoxy of oxirane value between 0.2 ~ 04 of the epoxy resin described in step (2).
5. the preparation method of a kind of laser sintered 3D printing technique nano-silicon nitride powder according to claim 1, is characterized in that, the mass ratio of the epoxy resin described in step (2) and pyromellitic dianhydride is optimum between 1:0.08 ~ 0.12.
6. the laser sintered 3D printing technique nano-silicon nitride powder prepared by preparation method of a kind of laser sintered 3D printing technique nano-silicon nitride powder according to claim 1, it is characterized in that, the condition of molding of described laser sintered 3D printing technique nano-silicon nitride powder is: laser power is 20 ~ 40W, sweep velocity is 1500mm/s, sweep span is 0.1 ~ 0.15mm, lift height is 0.10 ~ 0.2mm, preheating temperature: 50 DEG C, and processing temperature is 120 ~ 130 DEG C.
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| CN105195679A (en) * | 2015-09-21 | 2015-12-30 | 济南大学 | Preparing method for fast forming epoxy resin coated sand used for 3D printing |
| CN105215281A (en) * | 2015-09-21 | 2016-01-06 | 济南大学 | A kind of preparation method printing quartzy precoated sand for 3D |
| CN105254309A (en) * | 2015-09-24 | 2016-01-20 | 佛山华智新材料有限公司 | Ceramic 3D printing method |
| CN105367998A (en) * | 2015-11-20 | 2016-03-02 | 苏州光韵达光电科技有限公司 | Preparation method of 3D printing material |
| CN106380173A (en) * | 2016-09-07 | 2017-02-08 | 济南大学 | Preparation method of quick-forming black pottery powder for laser sintering 3D (three-dimensional) printing |
| CN108264356A (en) * | 2018-03-06 | 2018-07-10 | 济南大学 | One kind is molded TiB for 3DP2The preparation method of composite ceramic material |
| CN109761621A (en) * | 2019-03-18 | 2019-05-17 | 哈尔滨工业大学 | A kind of method preparing big-size complicated shape silicon nitride ceramics |
| US11577458B2 (en) | 2018-06-29 | 2023-02-14 | 3M Innovative Properties Company | Additive layer manufacturing method and articles |
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| CN105195679A (en) * | 2015-09-21 | 2015-12-30 | 济南大学 | Preparing method for fast forming epoxy resin coated sand used for 3D printing |
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| CN105367998A (en) * | 2015-11-20 | 2016-03-02 | 苏州光韵达光电科技有限公司 | Preparation method of 3D printing material |
| CN106380173A (en) * | 2016-09-07 | 2017-02-08 | 济南大学 | Preparation method of quick-forming black pottery powder for laser sintering 3D (three-dimensional) printing |
| CN108264356A (en) * | 2018-03-06 | 2018-07-10 | 济南大学 | One kind is molded TiB for 3DP2The preparation method of composite ceramic material |
| US11577458B2 (en) | 2018-06-29 | 2023-02-14 | 3M Innovative Properties Company | Additive layer manufacturing method and articles |
| CN109761621A (en) * | 2019-03-18 | 2019-05-17 | 哈尔滨工业大学 | A kind of method preparing big-size complicated shape silicon nitride ceramics |
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